CN106159204A - A kind of active substance growth in situ electrode slice and preparation method thereof - Google Patents

A kind of active substance growth in situ electrode slice and preparation method thereof Download PDF

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Publication number
CN106159204A
CN106159204A CN201610577249.8A CN201610577249A CN106159204A CN 106159204 A CN106159204 A CN 106159204A CN 201610577249 A CN201610577249 A CN 201610577249A CN 106159204 A CN106159204 A CN 106159204A
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China
Prior art keywords
electrode slice
source
situ
growth
active substance
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CN201610577249.8A
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Chinese (zh)
Inventor
张露露
李振
杨学林
孙华斌
丁晓凯
周英贤
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China Three Gorges University CTGU
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China Three Gorges University CTGU
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Priority to CN201610577249.8A priority Critical patent/CN106159204A/en
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
    • 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 present invention provides a kind of active substance growth in situ electrode slice, active material presoma homogeneous impregnation is coated on ordinary filter paper, again by the active material growth in situ of formation after calcining on the carbon fiber after filter paper carbonization as collector, gained active material is active substance growth in situ electrode slice with the composite of carbon fiber.Its method is that precursor powder is transferred in N methyl pyrrolidone (NMP) medium stir into slurry, then filter paper impregnation ultrasonic, dry, punching in slurry is obtained disk, disk is in tube furnace under inert atmosphere, 5 24h are sintered at 500 800 DEG C, obtain positive electrode growth in situ electrode slice on carbon fiber, i.e. active substance growth in situ electrode slice.Comparing general electrode slice preparation method, the present invention, with gained carbon fiber after filter paper carbonization as collector, utilizes the sintering process of active material to be done directly the making of electrode slice, enormously simplify cell making process, reduce battery cost of manufacture.

Description

A kind of active substance growth in situ electrode slice and preparation method thereof
Technical field
The present invention relates to electrode slice prepared by growth in situ and preparation method thereof, belong to the preparation neck of cell positive material Territory.
Background technology
Along with people's improving constantly the growing and social of energy demand and sustainable economic development, there is height The green energy resource of performance low cost causes the concern that people are the most.
Lithium ion battery owing to having that running voltage is high, specific energy is big, self discharge is little, have extended cycle life and environmental friendliness etc. Advantage, it has also become energy storing device ideal after twentieth century.In recent years, lithium ion battery is widely used to portable Formula electronic equipment, in terms of the electronic product such as notebook computer, mobile phone, future will become further in electric automobile, state The contenders of the power supplys such as anti-industry.Along with lithium ion battery is more and more extensive in the application of different field, every field pair The performance of lithium ion battery it is also proposed different requirements.
Existing lithium ion battery can be divided into takeup type and stacked two classes, and its structure mainly includes positive pole, negative pole, electrolysis Liquid, barrier film, shell and contact conductor.Wherein, positive pole and negative pole be all anode and cathode active materials is coated in the most positive and negative On the collector of pole.The electric current that cell active materials produces mainly is collected to form bigger electricity by the function of collector Stream externally output, therefore collector should be fully contacted with active substance, and internal resistance should be the least.Existing lithium ion battery In, collector generally uses foil, and as negative pole uses Copper Foil, and positive pole uses aluminium foil.But, these foils are general There is bigger weight, so that the energy density of lithium ion battery is less；Simultaneously as metal material is easily corroded, enter one Step have impact on the service life of lithium ion battery.And, first the preparation method of current lithium ion cell electrode is usually will live Property material mixes with conductive agent and binding agent, is then coated in conductive current collector by slurry.Material with carbon element and conductive agent and bonding The ratio of agent, the technique closing slurry and painting sizing process are the most complicated and the performance of electrode material is had large effect.
There is provided a kind of growth in situ electrode slice in consideration of it, necessary, the collector density of this electrode slice is less, be difficult to by Corrosion and synthesis technique are the simplest.
Summary of the invention
Compared to prior art, use in the preparation process of the electrode slice of described growth in situ positive electrode active materials is common After filter paper carbonization, main component is carbon fiber, and therefore, the weight of collector is less；Meanwhile, the carbon fiber afflux after growth in situ Body chemical stability is high, and therefore, collector is difficult to be corroded.Use the lithium ion of this growth in situ positive electrode active materials electrode slice Battery has higher energy density and longer service life cycle.This electrode slice manufacture method is in positive pole by filter paper impregnation Material precursor, with the mixed slurry of NMP, by sintering, makes positive active material growth in situ fine at filter paper carbonization gained carbon In dimension, this electrode slice can be directly used for assembled battery.The present invention, with gained carbon fiber after filter paper carbonization as collector, utilizes activity The sintering process of material is done directly the making of electrode slice, enormously simplify cell making process, reduces battery cost of manufacture.
It is an object of the invention to provide a kind of active substance growth in situ positive electrical pole piece, active material presoma is uniform Immersion coating is on ordinary filter paper, then makes on active material growth in situ carbon fiber after filter paper carbonization by sintering process, Gained active material is this growth in situ electrode slice with the composite of carbon fiber.
Another object of the present invention is to provide the manufacture method of a kind of active substance growth in situ electrode slice, this preparation Method is directly with gained carbon fiber after filter paper carbonization as collector, and owing to carbon fiber density is little, chemical stability is high, therefore this is former Position growth electrode slice has higher energy density and more excellent cycle performance.
For reaching above-mentioned purpose, a kind of active substance growth in situ electrode slice, including lithium source, vanadium source and/or source of iron, phosphorus source And filter paper；Filter paper uses agent treated remove impurity；Lithium source, vanadium source and/or source of iron, phosphorus source prepares positive pole by certain mixed in molar ratio Material precursor；The thing of composite is pure phase mutually.
As materialization, the purity of described lithium source, vanadium source and/or source of iron and phosphorus source is all higher than 99%.
For reaching above-mentioned another object, the present invention provides the preparation method of a kind of active substance growth in situ electrode slice, will Filter paper soaks 1-24h through hydrochloric acid reagent and carries out remove impurity, obtains pure cellulose tissue after rinsing；
Again by lithium source Li2CO3, source of iron Fe2O3And/or vanadium source NH4VO3, phosphorus source NH4H2PO4Ball milling 10h in anhydrous ethanol medium After, transfer in the baking oven of 50 ° of C be dried 12h, gained powder in tube furnace at 250-400 DEG C pre-burning 3-12h, obtain pre- Burn product；
Then in pre-burning product, add carbon source, with dehydrated alcohol for medium ball milling 6h, after drying, obtain precursor powder；
It is transferred to precursor powder further N-Methyl pyrrolidone (NMP) medium stirs into slurry, then filter paper is soaked Stain is ultrasonic in slurry, dry, punching obtains disk；
Finally disk under inert atmosphere, is sintered at 500-800 DEG C 5-24h, obtains positive electrode the most raw in tube furnace Long electrode slice on carbon fiber, i.e. active substance growth in situ electrode slice.
Described lithium source Li2CO3, source of iron Fe2O3And/or vanadium source NH4VO3, phosphorus source NH4H2PO4Mol ratio be 1.5:2:3.
Described carbon source is organic carbon source or inorganic carbon source, and its addition accounts for the 1 ~ 20% of raw material gross mass, specifically includes Glucose, sucrose, ascorbic acid, citric acid, oxalic acid, acetylene black, CNT, Super P, polyvinyl alcohol, Polyethylene Glycol, shallow lake One or more in powder；Described medium is acetone, ethanol or aqueous solvent.
Described inert atmosphere includes nitrogen, argon or argon hydrogen gaseous mixture.
Positive electrode growth in situ electrode slice of the present invention has a following advantage:
(1) this growth in situ electrode slice has the chemical property of excellence, and specific capacity and cycle performance are significantly improved, electrode Stability and the energy density of sheet are greatly increased；(2) comparing general electrode slice preparation method, the present invention is with institute after filter paper carbonization Obtaining carbon fiber is collector, utilizes the sintering process of active material to be done directly the making of electrode slice, enormously simplify battery system Make technique, reduce battery cost of manufacture.
The present invention prepares the method for high-performance positive electrode growth in situ electrode slice on carbon fiber and has following Distinguishing feature:
(1) with low cost, pollution-free；
(2) in building-up process, noxious gas emission is few；
(3) resulting materials electrochemical performance.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of sample in presoma, embodiment 1 and comparative example 1.
Fig. 2 is the stereoscan photograph of sample in embodiment 1.
Fig. 3 is the charging and discharging curve of sample in comparative example 1 and embodiment 1.
Fig. 4 is the cycle performance curve of sample in comparative example 1 and embodiment 1.
Detailed description of the invention
Below by embodiment and the description of comparative example, substantive distinguishing features and the advantage of the present invention are expanded on further.For retouching State conveniently, first comparative example is described, describe embodiment the most again, compare therewith, demonstrate the effect of the present invention.Below Described is the preferred embodiment of the present invention, it is noted that for those skilled in the art, without departing from On the premise of the principle of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as the protection of the present invention Scope.
Comparative example 1
Medicine and the mol ratio of preparing sample needs meet following relation: by Li2CO3、NH4VO3、NH4H2PO4With mol ratio it is 1.5:2:3 is transferred in the baking oven of 50 ° of C be incubated about 12 h after ball milling 10h mixing in anhydrous ethanol medium, to be dried after in Lower 350 ° of C pre-burning 6 h of nitrogen atmosphere in tube furnace.It is that the glucose of 10% is at dehydrated alcohol by the powder obtained and mass fraction Ball milling 6 h in medium, obtains precursor powder after drying.Presoma in tube furnace under nitrogen atmosphere 700 ° of C be sintered, Sintering time 10 h, sieves, and obtains sample LVP/C.By active substance LVP/C with acetylene black, Kynoar (PVdF) by 75: The mass ratio of 15:10 is furnishing slurry in N-Methyl pyrrolidone (NMP) medium, coats on aluminium foil, through being dried, rush film and Press mold makes working electrode.With lithium metal for electrode, Celgard 2400 is barrier film, 1M LiPF6/(EC+DMC) (1:1) Being assembled into battery for electrolyte and carry out constant current charge-discharge test, voltage range is between 3.0 ~ 4.3 V.Material 1 C discharges first Capacitance is 116.9 mAh g-1, after 500 circulations, discharge capacity maintains 113.5 mAh g-1, capability retention is only 97.09%。
Embodiment 1
It is 12 hours that ordinary filter paper is used hydrochloric acid reagent remove impurity, process time, afterwards by filter paper rinsed clean.By Li2CO3、 NH4VO3、NH4H2PO4In anhydrous ethanol medium, the baking oven of 50 ° of C after ball milling 10h mixing, it is transferred to mol ratio for 1.5:2:3 Middle insulation about 12 h, to be dried after in tube furnace lower 350 ° of C pre-burning 6 h of nitrogen atmosphere, obtain pre-burning product, pre-burning product Middle addition mass fraction be 10% glucose sugar as organic carbon source, with dehydrated alcohol for medium ball milling 6h, 50 DEG C of drying obtain Precursor powder.It is transferred to precursor powder in N-Methyl pyrrolidone (NMP) medium stir into slurry, then filter paper is soaked Stain is ultrasonic in slurry, and 80 DEG C of dry, punchings, disk carries out 700 DEG C of sintering in tube furnace under inert atmosphere (blanket of nitrogen) 10h, naturally cools to room temperature, obtains positive electrode growth in situ electrode slice on carbon fiber.With lithium metal for electrode, Celgard 2400 is barrier film, 1M LiPF6/ (EC+DMC) (1:1) is that electrolyte is assembled into battery and carries out constant current charge-discharge survey Examination, voltage range is between 3.0 ~ 4.3 V.Material 1 C discharge capacity first is 123.9 mAh g-1, after 500 times circulate Discharge capacity maintains 122.8 mAh g-1, capability retention is 99.11%.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as Protection scope of the present invention.

Claims (7)

1. an active substance growth in situ electrode slice, it is characterised in that active material presoma homogeneous impregnation is coated in commonly On filter paper, then by the active material growth in situ of formation after calcining on the carbon fiber after filter paper carbonization as collector, institute The composite obtaining active material and carbon fiber is active substance growth in situ electrode slice.
2. the active substance growth in situ electrode slice described in claim 1, it is characterised in that described filter paper is by cellulose structure Become, after high temperature cabonization, form the carbon fiber with porous carbon fiber structure.
3. the active substance growth in situ electrode slice described in claim 1, it is characterised in that described active material presoma is Positive electrode material precursor, including preparing the presoma of phosphoric acid vanadium lithium, preparing the presoma of LiFePO4, specially lithium source Li2CO3, Source of iron Fe2O3And/or vanadium source NH4VO3, phosphorus source NH4H2PO4。
4. the preparation method of the active substance growth in situ electrode slice described in any one of claim 1-3, it is characterised in that include Following steps:
(1) filter paper is soaked 1-24h through hydrochloric acid reagent and carry out remove impurity, after rinsing, obtain pure cellulose tissue；
By lithium source Li2CO3, source of iron Fe2O3And/or vanadium source NH4VO3, phosphorus source NH4H2PO4In anhydrous ethanol medium after ball milling 10h, Transfer in the baking oven of 50 ° of C be dried 12h, gained powder in tube furnace at 250-400 DEG C pre-burning 3-12h, obtain pre-burning produce Thing；
(2) in pre-burning product, add carbon source, with dehydrated alcohol for medium ball milling 6h, after drying, obtain precursor powder；
It is transferred to precursor powder in N-Methyl pyrrolidone (NMP) medium stir into slurry, then by filter paper impregnation in slurry In material, ultrasonic, dry, punching obtains disk；
(3) disk under inert atmosphere, sinters 5-24h at 500-800 DEG C, obtains positive electrode growth in situ and exist in tube furnace Electrode slice on carbon fiber, i.e. active substance growth in situ electrode slice.
5. the preparation method of the active substance growth in situ electrode slice described in claim 4, it is characterised in that lithium in step (2) Source Li2CO3, source of iron Fe2O3And/or vanadium source NH4VO3, phosphorus source NH4H2PO4Mol ratio be 1.5:2:3.
6. the preparation method of the active substance growth in situ electrode slice described in claim 4, it is characterised in that step (3) is described Carbon source be organic carbon source or inorganic carbon source, its addition accounts for the 1 ~ 20% of raw material gross mass, specifically include glucose, sucrose, One in ascorbic acid, citric acid, oxalic acid, acetylene black, CNT, Super P, polyvinyl alcohol, Polyethylene Glycol, starch or Several；Described medium is acetone, ethanol or aqueous solvent.
7. the preparation method of the active substance growth in situ electrode slice described in claim 4, it is characterised in that institute in step (5) The inert atmosphere stated includes nitrogen, argon or argon hydrogen gaseous mixture.
CN201610577249.8A 2016-07-21 2016-07-21 A kind of active substance growth in situ electrode slice and preparation method thereof Pending CN106159204A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107317036A (en) * 2017-06-27 2017-11-03 中南大学 A kind of pole piece with super-low resistance, its preparation method and the lithium ion battery containing this pole piece
CN107819149A (en) * 2017-11-09 2018-03-20 天津工业大学 A kind of method that growth in situ prepares all-solid sodium ion battery
CN108455561A (en) * 2018-05-02 2018-08-28 东北林业大学 A kind of preparation method of paper substrate mesoporous carbon electrode material and the preparation method of electrode
CN108807909A (en) * 2018-06-13 2018-11-13 深圳汽航院科技有限公司 A kind of preparation method of flexible composite, water system nickel iron cell electrode and battery comprising the flexible composite
CN111600001A (en) * 2020-05-30 2020-08-28 海宏(唐河)新能源科技有限公司 Preparation method of capacitance lithium iron carbonate phosphate composite material
CN111684624A (en) * 2017-12-08 2020-09-18 荷兰应用自然科学研究组织Tno Low temperature preparation of cathode active materials
CN114613945A (en) * 2022-04-02 2022-06-10 北京师范大学 Preparation method of lithium ion battery anode

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102244241A (en) * 2011-05-31 2011-11-16 合肥国轩高科动力能源有限公司 Preparation method of lithium iron phosphate composite material modified by lithium pyrophosphate
CN105762337A (en) * 2016-01-22 2016-07-13 三峡大学 Silicon/graphene/carbon fiber composite cathode material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102244241A (en) * 2011-05-31 2011-11-16 合肥国轩高科动力能源有限公司 Preparation method of lithium iron phosphate composite material modified by lithium pyrophosphate
CN105762337A (en) * 2016-01-22 2016-07-13 三峡大学 Silicon/graphene/carbon fiber composite cathode material and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107317036A (en) * 2017-06-27 2017-11-03 中南大学 A kind of pole piece with super-low resistance, its preparation method and the lithium ion battery containing this pole piece
CN107317036B (en) * 2017-06-27 2021-03-02 中南大学 Pole piece with ultralow resistance, preparation method thereof and lithium ion battery containing pole piece
CN107819149A (en) * 2017-11-09 2018-03-20 天津工业大学 A kind of method that growth in situ prepares all-solid sodium ion battery
CN111684624A (en) * 2017-12-08 2020-09-18 荷兰应用自然科学研究组织Tno Low temperature preparation of cathode active materials
CN111684624B (en) * 2017-12-08 2024-03-15 荷兰应用自然科学研究组织Tno Low temperature preparation of cathode active material
CN108455561A (en) * 2018-05-02 2018-08-28 东北林业大学 A kind of preparation method of paper substrate mesoporous carbon electrode material and the preparation method of electrode
CN108455561B (en) * 2018-05-02 2021-10-29 东北林业大学 Preparation method of paper-based mesoporous carbon electrode material and preparation method of electrode
CN108807909A (en) * 2018-06-13 2018-11-13 深圳汽航院科技有限公司 A kind of preparation method of flexible composite, water system nickel iron cell electrode and battery comprising the flexible composite
CN108807909B (en) * 2018-06-13 2021-02-12 深圳汽航院科技有限公司 Preparation method of flexible composite material, water system nickel-iron battery electrode containing flexible composite material and battery
CN111600001A (en) * 2020-05-30 2020-08-28 海宏(唐河)新能源科技有限公司 Preparation method of capacitance lithium iron carbonate phosphate composite material
CN114613945A (en) * 2022-04-02 2022-06-10 北京师范大学 Preparation method of lithium ion battery anode
CN114613945B (en) * 2022-04-02 2023-06-23 北京师范大学 Preparation method of positive electrode of lithium ion battery

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Application publication date: 20161123