CN108933253A - A kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material - Google Patents

A kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material Download PDF

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Publication number
CN108933253A
CN108933253A CN201811084542.6A CN201811084542A CN108933253A CN 108933253 A CN108933253 A CN 108933253A CN 201811084542 A CN201811084542 A CN 201811084542A CN 108933253 A CN108933253 A CN 108933253A
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China
Prior art keywords
temperature
ion battery
lithium ion
negative electrode
electrode material
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CN201811084542.6A
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Chinese (zh)
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罗大为
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Shenzhen Polytechnic
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Shenzhen Polytechnic
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Priority to CN201811084542.6A priority Critical patent/CN108933253A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

A kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material includes the following steps: step 1: weighing the Le cuckoo petal that 4.0g is newly picked and being soaked in volumetric concentration is 25% ammonia spirit 48h, three times with deionized water and washes of absolute alcohol, is then filtered and dry;Step 2: the Le cuckoo petal through AMMONIA TREATMENT immerses 100mL ethylene glycol, is subsequently added into 2.0g polyethylene glycol 400, and FeCl is added3·6H2Dissolution and ultrasonication 1h is sufficiently stirred in O and sodium acetate (NaAc);Step 3: step 2 acquired solution being transferred in polytetrafluoroethyllining lining, 16h is kept the temperature at 200 DEG C, is cooled to room temperature, is washed three times with deionized water and dehydrated alcohol, is put into 80 DEG C of vacuum ovens and keeps the temperature 8h, drying is stand-by;Step 4: the mixture that step 3 is obtained is placed in crucible, under high-purity argon gas protection, is warming up to certain temperature with 10 DEG C/min speed, and keep the temperature 6h, slow cooling to room temperature.Anode material capacity height of the present invention and good cycle have application prospect in the fields such as portable electronic device and electric car.

Description

A kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material
Technical field
The present invention relates to lithium ion battery negative material fields, and in particular to a kind of lithium ion battery Fe2O3/ C negative electrode material Preparation method.
Background technique
Lithium ion battery is the novel secondary chemical energy storage device of a kind of great potential, is widely used in portable electronic The fields such as equipment, electric vehicle and smart grid.The design and synthesis of high performance electrode material be obtain high-energy density, The key of long circulation life, high security lithium ion battery.Currently, negative electrode material of the graphite carbon material as lithium ion battery Application than wide, but since to store up lithium ability lower for it, be not able to satisfy the demand of large capacity, high power lithium ion cell, at For the bottleneck for limiting lithium battery capacity.The space for improving its capacity is very limited, and graphite-based carbon cathode can be substituted by finding one kind Material, the novel secondary lithium ion battery negative material with higher capacity and safety be urgent and necessary.
For iron oxide as lithium ion battery negative material there are many prominent advantage, theoretical capacity is significantly larger than nowadays quotient The graphite material of industry, and iron oxide is resourceful, and cheap, nonhazardous, theoretical specific capacity is up to 1005mAh/ G, these advantages determine that iron oxide is a kind of lithium ion battery negative material for having very much potential application, at novel in recent years The hot spot of negative electrode material research.But as a kind of lithium ion battery negative material, some defects are equally existed, such as iron oxide sheet The electric conductivity of body is poor, and iron oxide cathode material volume change in charge and discharge process is significant, and structural stability is poor, and circulation is held Amount decline is quickly.
Summary of the invention
The technical problem to be solved in the present invention is that: at present lithium cell cathode material there are capacity is not high and cycle performance not Ideal problem proposes a kind of lithium ion battery Fe2O3The preparation method of/C composite negative pole material improves electrode cycle and stablizes Property, and the lithium ion battery negative material of high capacity high stability is prepared, and then improve the globality of power lithium-ion battery Energy.
In order to solve the above-mentioned technical problem, the present invention proposes a kind of following technical scheme: lithium ion battery Fe2O3/ C cathode The preparation method of material, includes the following steps:
Step 1: weighing the Le cuckoo petal that 4.0g is newly picked and being soaked in volumetric concentration is 25% ammonia spirit 48h, is spent Ionized water and washes of absolute alcohol three times, then filter and dry;
Step 2: the Le cuckoo petal through AMMONIA TREATMENT immerses 100mL ethylene glycol, is subsequently added into 2.0g polyethylene glycol, then The FeCl of certain mass is added3·6H2Dissolution and ultrasonication 1h is sufficiently stirred in O and sodium acetate;
Step 3: step 2 acquired solution being transferred in polytetrafluoroethyllining lining, 16h is kept the temperature at 200 DEG C, is cooled to room Temperature is then washed three times with deionized water and dehydrated alcohol respectively, is put into 80 DEG C of vacuum ovens and is kept the temperature 8h, and drying is stand-by;
Step 4: the mixture that step 3 is obtained is placed in crucible, then under high-purity argon gas protection, with 10 DEG C/min speed Degree is warming up to certain temperature, and keeps the temperature 6h, and then slow cooling to room temperature is to get to lithium ion battery Fe2O3/ C negative electrode material.
The above technical solution is further limited in that: in step 2, FeCl is added3·6H2The quality control of O 1~ Between 3g, the quality of sodium acetate is controlled between 8~10g.
The above technical solution is further limited in that: in step 4, it is warming up between 600~800 DEG C.
Compared with prior art, the present invention has following the utility model has the advantages that the present invention is made a living object template with strangling cuckoo petal, fills Divide and utilize petal network abundant, Fe can be effectively adsorbed after being impregnated to it with ammonium hydroxide3+, when using hydrothermal synthesis method, A large amount of Fe can be loaded in petal surface2O3Particle, and petal is Fe after high temperature cabonization under protection of argon gas2O3Particle provides conductive Access greatly strengthens Fe2O3The electric conductivity of/C composite negative pole material, and then improve the overall performance of power lithium-ion battery.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite negative pole material of the embodiment of the present invention 1.
Fig. 2 is the cycle performance figure of the composite negative pole material of the embodiment of the present invention 1.
Specific embodiment
The various parameters of 1-4 of the embodiment of the present invention are as shown in table 1.
Parameter in the different embodiments of table 1
The present invention is explained with embodiment 1.The preparation process of embodiment 2 to embodiment 4 is the preparation with embodiment 1 Cheng Xiangtong, it is only necessary to adjust according to parameter in table 1.
Weighing the Le cuckoo petal that 4.0g is newly picked and being soaked in volumetric concentration is 25% ammonia spirit 48h, uses deionized water Three times with washes of absolute alcohol, it then filters and dry.Le cuckoo petal through AMMONIA TREATMENT immerses 100mL ethylene glycol, then It is added 2.0g polyethylene glycol 400 (PEG 400), it is 2.0g FeCl that quality, which is then added,3·6H2O and quality are 8.5g sodium acetate (NaAc), dissolution and ultrasonication 1h is sufficiently stirred.
Above-mentioned solution is transferred in polytetrafluoroethyllining lining, 16h is kept the temperature at 200 DEG C, is cooled to room temperature.Then distinguish It is washed three times with deionized water and dehydrated alcohol, is put into 80 DEG C of vacuum ovens and keeps the temperature 8h drying.
The mixture of above-mentioned drying is placed in crucible, then under high-purity argon gas protection, with the heating of 10 DEG C/min speed To 750 DEG C, and keep the temperature 6h, then slow cooling to room temperature to get arrive Fe2O3/ C composite negative pole material.
Electrochemical property test is carried out to obtained composite negative pole material, the results showed that, in 100mAg-1Current density Under, discharge capacity is 1223.7mAhg to composite material for the first time-1, 50 times circulation after reversible capacity can still maintain 694.0mAh g-1, there is preferable chemical property.

Claims (3)

1. a kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material, which comprises the steps of:
Step 1: weighing the Le cuckoo petal that 4.0 g are newly picked and be soaked in 48 h in the ammonia spirit that volumetric concentration is 25%, use Deionized water and washes of absolute alcohol three times, then filter and dry;
Step 2: the Le cuckoo petal through AMMONIA TREATMENT immerses 100mL ethylene glycol, is subsequently added into 2.0 g polyethylene glycol 400s, then The FeCl of certain mass is added3·6H2Dissolution and ultrasonication 1h is sufficiently stirred in O and sodium acetate;
Step 3: step 2 acquired solution is transferred in polytetrafluoroethyllining lining, 16h is kept the temperature at 200 DEG C, is cooled to room temperature, Then it is washed three times with deionized water and dehydrated alcohol respectively, is put into 80 DEG C of vacuum ovens and keeps the temperature 8h, drying is stand-by;
Step 4: the mixture that step 3 is obtained is placed in crucible, then under high-purity argon gas protection, with 10 DEG C/min speed liter Temperature arrives certain temperature, and keeps the temperature 6h, and then slow cooling to room temperature is to get to lithium ion battery Fe2O3/ C negative electrode material.
2. a kind of lithium ion battery Fe according to claim 12O3The preparation method of/C negative electrode material, it is characterised in that: step In rapid 2, FeCl is added3·6H2The quality of O controls between 1 ~ 3g, and the quality of sodium acetate controls between 8 ~ 10g.
3. a kind of lithium ion battery Fe according to claim 12O3The preparation method of/C negative electrode material, it is characterised in that: step In rapid 4, it is warming up between 600 ~ 800 DEG C.
CN201811084542.6A 2018-09-17 2018-09-17 A kind of lithium ion battery Fe2O3The preparation method of/C negative electrode material Pending CN108933253A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208614A (en) * 2011-04-26 2011-10-05 中国矿业大学 Method for preparing lithium ion battery cathode material coated iron sesquioxide
CN107026266A (en) * 2017-06-05 2017-08-08 深圳职业技术学院 A kind of lithium ion battery CNTs/Fe2O3The preparation method of/C composite negative pole materials
CN107039635A (en) * 2017-04-20 2017-08-11 陕西科技大学 A kind of preparation method of FeOOH/biomass carbon sodium-ion battery self-supporting negative pole

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102208614A (en) * 2011-04-26 2011-10-05 中国矿业大学 Method for preparing lithium ion battery cathode material coated iron sesquioxide
CN107039635A (en) * 2017-04-20 2017-08-11 陕西科技大学 A kind of preparation method of FeOOH/biomass carbon sodium-ion battery self-supporting negative pole
CN107026266A (en) * 2017-06-05 2017-08-08 深圳职业技术学院 A kind of lithium ion battery CNTs/Fe2O3The preparation method of/C composite negative pole materials

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YAN SUN ET.AL: "Spinach juice-derived porous Fe2O3/carbon nanorods as superior anodes for lithium-ion batteries", 《MATERIALS RESEARCH BULLETIN》 *
张苏月: "FexOy及其复合物锂离子电池负极材料的生物模板法制备与性能", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

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Application publication date: 20181204

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