CN107611414A - A kind of preparation method of anode material for lithium-ion batteries - Google Patents
A kind of preparation method of anode material for lithium-ion batteries Download PDFInfo
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- CN107611414A CN107611414A CN201711026496.XA CN201711026496A CN107611414A CN 107611414 A CN107611414 A CN 107611414A CN 201711026496 A CN201711026496 A CN 201711026496A CN 107611414 A CN107611414 A CN 107611414A
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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 present invention is by electric current auxiliary positive material preparation method, by being aided with electric current while sintering, so as to less than under nominal sintering temperatures, obtain anode material for lithium-ion batteries, it can be widely applied in the preparation of various anode material for lithium-ion batteries.The furnace temperature that the present invention is prepared needed for positive electrode is low (200 1000 DEG C), and power consumption is low.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, belong to field of lithium ion battery.
Background technology
Lithium ion battery is a kind of novel high-energy green secondary cell, it has, and capacity is high, voltage is high, have extended cycle life,
The advantages that security is good, obtained extensively in every field such as portable electric appts, electric automobile, space technology, national defense industry
General use.Lithium ion battery is made up of positive pole, negative pole, barrier film, positive electrode, collector etc..Cell reaction is：Charging
Cheng Zhong, Li+Deviate from from positive pole, discharge an electronics, while transition metal ions aoxidizes, Li+Reached by positive electrode negative
Pole, embedded negative material, electronics flow to negative pole by external circuit by positive pole；During electric discharge, Li+Deviate from from negative pole, pass through positive pole material
In the embedded positive electrode of material, reduction reaction occurs for transition metal ions, and electronics is deviate from from negative pole, reaches positive pole by external circuit.
At present, the capacity of the positive electrode of lithium ion battery turn into limiting lithium ion cell capacity bottleneck, and lithium ion anode into
Originally a big chunk of lithium ion battery cost is also taken up.
The preparation method of anode material for lithium-ion batteries mainly has solid phase method, coprecipitation, sol-gal process etc. at present,
It is required for very high furnace temperature to be sintered material in these preparation methods, such as LiCoO2Material needs to burn under 900 DEG C of furnace temperature
Knot, Li1Ni1/3Co1/3Mn1/3O2Need to sinter under 800 DEG C of furnace temperature.And some new materials are also difficult under very high furnace temperature
With synthesis, such as Li1.2Fe0.4Zr0.4O2All it is difficult to synthesize at 1300 DEG C.
The content of the invention
The invention aims to solve existing prepare to be difficult to reach institute in anode material for lithium-ion batteries sintering process
A kind of high-temperature problem needed, there is provided method that anode material for lithium-ion batteries is prepared under relatively low furnace temperature.
The present invention is by electric current auxiliary positive material preparation method, by being aided with electric current while sintering, so as to
Less than under nominal sintering temperatures, anode material for lithium-ion batteries is obtained, it can be widely applied to various lithium ion cell positives
In the preparation of material.
The present invention provides a kind of preparation method of anode material for lithium-ion batteries, comprises the following steps：
(1) precursor of lithium ionic cell positive material powder is proportionally weighed, makes it well mixed；
(2) positive electrode material precursor after will be well mixed is suppressed；
(3) by the positive electrode material precursor both ends series connection access circuit after compacting, it is subsequently placed in incinerator, is heating up
While at positive electrode material precursor both ends apply 10V cm-1~400V cm-1Electric field, pass through positive electrode forerunner when there is electric current
When in body, keeping temperature, by the Maximum constraint of current density in 10mA mm-2~1000mA mm-2, it is high to carry out electric current auxiliary
Temperature synthesis, is kept for the constant current density and heat preservation sintering certain time, obtains anode material for lithium-ion batteries；Or
By in the positive electrode material precursor both ends series connection access circuit after compacting, it is subsequently placed in incinerator, is warming up to institute
Temperature is needed, then applying both ends to positive electrode material precursor applies 10V cm-1~400V cm-1(the electricity applied in unit length
Pressure) electric field is until produce electric current, and by the Maximum constraint of current density in 10mA mm-2~1000mA mm-2, carry out electric current
Assisted with high-temperature synthesizes, and is kept for the constant current density and heat preservation sintering certain time, obtains anode material for lithium-ion batteries.
Preparation in accordance with the present invention, the precursor of lithium ionic cell positive material include：Lithium source, source metal.Lithium
Source is selected from compound or composition containing lithium, is preferably selected from lithium hydroxide, lithium nitrate, lithium carbonate, lithium oxalate, lithium fluoride, bromination
One or more in lithium, lithium chloride, lithium acetate, lithia, lithium dihydrogen phosphate and lithium phosphate, be more preferably selected from lithium hydroxide and
Lithium carbonate.Source metal be selected from aluminium, magnesium, calcium, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, gallium, germanium, rubidium, strontium, yttrium, zirconium, niobium,
Molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, barium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, lanthanide series, actinides
One or more in oxide, hydroxide, carbonate, oxalates, nitrate, fluoride and chloride.
Preparation in accordance with the present invention, the positive electrode material precursor can use sol-gal process, hydro-thermal method, solid phase
It is prepared by synthetic method, method of electrostatic spinning, microemulsion method or coprecipitation；The hybrid mode can include ball milling mixing, grinding mixes
Conjunction, ultrasonic mixing, collosol and gel mixing；
Preparation in accordance with the present invention, the compacting of the positive electrode material precursor can use conventional compacting tool set to enter
Row compacting, and it is possible to not be removed from the molds the positive electrode material precursor after compacting after pressing, directly in mould
In the presence of, in the both ends series connection access circuit of positive electrode material precursor after pressing.The pressing pressure of mould is preferably
0.1MPa to 100MPa, more preferably 0.1MPa are to 10MPa.It is specific as follows：
Well mixed positive electrode material precursor is added in mould, and suppressed, by the positive pole material in mould after compacting
In material precursor series connection access circuit；Then mould is integrally placed in stove, started to warm up from room temperature, while starting to warm up
Apply electric field at positive electrode material precursor both ends, electric-field intensity is adjustable, from 10V cm-1~400V cm-1；Pass through when there is electric current
When in positive electrode material precursor, keeping temperature, by the Maximum constraint of current density in 10mA mm-2~1000mA mm-2, enter
Row electric current assisted with high-temperature synthesizes；Kept for the constant current density and heat preservation sintering certain time, obtain lithium ion cell positive material
Material；Or
Well mixed positive electrode material precursor is added in mould, and suppressed, by the positive pole material in mould after compacting
In material precursor series connection access circuit；Then mould is integrally placed in stove, started to warm up from room temperature, when temperature is raised to required temperature
When spending, steady temperature is kept until positive electrode material precursor is consistent with furnace body temperature, then to positive electrode material precursor application electricity
, electric-field intensity is adjustable, from 10V cm-1~400V cm-1Until producing electric current, now electric current can rise rapidly, and electric current is close
The Maximum constraint of degree is in 10mA mm-2~1000mA mm-2, carry out electric current assisted with high-temperature synthesis；Keep the constant current density
And heat preservation sintering certain time, obtain anode material for lithium-ion batteries.
According to the preparation of the present invention, core of the invention is electric current auxiliary synthesis, and required sintering temperature is low during synthesis
In the sintering temperature of routine, those skilled in the art are according to the teachings of the present invention, for different lithium ion anode material forerunners
Body, can be with the preference temperature and sintering time needed for unrestricted choice, generally in 200-1000 DEG C of scope by the experiment of routine.
In addition, for different lithium ion anode material presomas, used electric current and voltage also may be used when electric current assisted with high-temperature synthesizes
Selected within the scope of the invention with the experiment by routine, it does not form the limitation of the present invention.
The beneficial effects of the invention are as follows：The present invention is a kind of preparation method of anode material for lithium-ion batteries, and it passes through electricity
Assisted sintering is flowed, can be obtained all kinds of anode material for lithium-ion batteries less than under nominal sintering temperatures, prepare positive electrode institute
The furnace temperature needed is low (200-1000 DEG C), and power consumption is low.
Brief description of the drawings
Fig. 1 is that embodiment 1 sinters LiCoO after 5h at 230 DEG C2XRD；
Fig. 2 is that embodiment 1 sinters LiCoO after 5h at 230 DEG C2SEM figure；
Fig. 3 is that embodiment 2 sinters LiNi after 5h at 300 DEG C1/3Co1/3Mn1/3O2XRD；
Fig. 4 is that embodiment 2 sinters LiNi after 5h at 300 DEG C1/3Co1/3Mn1/3O2SEM figure；
Fig. 5 is that embodiment 3 sinters LiFePO after 2h at 380 DEG C4XRD；
Fig. 6 is that embodiment 3 sinters LiFePO after 2h at 380 DEG C4SEM figure；
Fig. 7 is that embodiment 3 sinters Li after 10min at 600 DEG C1.2Fe0.4Zr0.4O2XRD；
Fig. 8 is that embodiment 3 sinters Li after 10min at 600 DEG C1.2Fe0.4Zr0.4O2SEM figure.
Embodiment
For present disclosure, substantive features and marked improvement is expanded on further, following examples detailed description is hereby enumerated
It is as follows, but the present invention is not limited to following examples.
Embodiment 1
By LiCoO2(LCO) stoichiometric proportion of molecular formula weighs Li2CO3、Co2O3, add ethanol, ball milling 10h, after drying
LCO positive electrode material precursor powders are obtained, grinding is uniform, and mould is put into after drying, and is suppressed, and passes through mould two after compacting
The wire at end applies electric field to presoma powder.Then mould is placed in tube furnace, with 5 DEG C of min-1Heating rate by stove
Temperature from room temperature rises to 230 DEG C, steady temperature after temperature is raised to 230 DEG C, by constant external power supply to LCO positive electrode forerunners
Body applies 70V cm-1Electric field, carry out electric current assisted with high-temperature synthesis, while electric current can change rapidly；Control electric current rises to
27mA mm-2, keep furnace temperature and in 27mA mm-2Lower constant current sinters 2h, is then cut off circuit and furnace temperature is naturally cooled into room
Temperature, then obtain LCO positive electrodes.Fig. 1 is the XRD of LCO positive electrodes after sintering.Fig. 2 is LCO positive electrodes after sintering
SEM schemes.The characteristic peak shown by XRD we can show that LCO positive electrodes have been prepared out.
Embodiment 2
By LiNi1/3Co1/3Mn1/3O2(LNCMO) stoichiometric proportion of molecular formula weighs Li2CO3、NiCO3, CoO, MnO, add
Enter ethanol, ball milling 10h, LNCMO positive electrode material precursor powders are obtained after drying, grinding is uniform, is put into mould after drying, goes forward side by side
Row compacting, electric field is applied to presoma powder by the wire of both mold ends after compacting.Then mould is placed in tube furnace,
With 5 DEG C of min-1Heating rate furnace temperature is risen to 300 DEG C from room temperature, steady temperature after temperature is raised to 300 DEG C, by constant
External power supply applies 70V cm to LNCMO positive electrode material precursors-1Field strength, carry out electric current assisted with high-temperature synthesis, while electric current
It can change rapidly；Control electric current rises to 27mA mm-2, keep furnace temperature and in 27mA mm-2Lower constant current sinters 2h, is then cut off
Furnace temperature is simultaneously naturally cooled to room temperature by circuit, then obtains LNCMO positive electrodes.Fig. 3 is the XRD of LNCMO positive electrodes after sintering
Figure.Fig. 4 is the SEM figures of LNCMO positive electrodes after sintering.The characteristic peak shown by XRD we can draw LNCMO positive poles
Material has been prepared out.
Embodiment 3
By LiFePO4(LFPO) stoichiometric proportion of molecular formula weighs Li2CO3、FeC2O4、NH4H2PO4, add ethanol, ball
10h is ground, LFPO positive electrode material precursor powders are obtained after drying, grinding is uniform, and mould is put into after drying, and is suppressed, and presses
Electric field is applied to presoma powder by the wire of both mold ends after system.Then mould is placed in tube furnace, with 5 DEG C
min-1Heating rate furnace temperature is risen to 380 DEG C from room temperature, steady temperature after temperature is raised to 380 DEG C, pass through constant external electricity
Source applies 100V cm to LFPO positive electrode material precursors-1Field strength, carry out electric current assisted with high-temperature synthesis, while electric current can be rapid
Change；Control electric current rises to 27mA mm-2, keep furnace temperature and in 27mA mm-2Lower constant current sinters 2h, is then cut off circuit simultaneously
Furnace temperature is naturally cooled into room temperature, then obtains LFPO positive electrodes.Fig. 5 is the XRD of LFPO positive electrodes after sintering.Fig. 6 is
The SEM figures of LFPO positive electrodes after sintering.The characteristic peak shown by XRD we can draw LFPO positive electrodes by
Prepare.
Embodiment 4
By Li1.2Fe0.4Zr0.4O2(LFZO) stoichiometric proportion of molecular formula weighs Li2CO3、Fe2O3、ZrO2, ethanol is added,
Ball milling 10h, LFZO positive electrode material precursor powders being obtained after drying, grinding is uniform, and mould is put into after drying, and is suppressed,
Electric field is applied to presoma powder by the wire of both mold ends after compacting.Then mould is placed in tube furnace, with 5 DEG C
min-1Heating rate furnace temperature is risen to 600 DEG C from room temperature, steady temperature after temperature is raised to 600 DEG C, pass through constant external electricity
Source applies 120V cm to LFZO positive electrode material precursors-1Field strength, carry out electric current assisted with high-temperature synthesis, while electric current can be rapid
Change；Control electric current rises to 135mA mm-2, keep furnace temperature and in 135mA mm-2Lower constant current sinters 10min, is then cut off electricity
Furnace temperature is simultaneously naturally cooled to room temperature by road, then obtains LFZO positive electrodes.Fig. 7 is the XRD of LFZO positive electrodes after sintering.Figure
8 scheme for the SEM of LFZO positive electrodes after sintering.The characteristic peak shown by XRD we can draw LFZO positive electrodes
Through being prepared out.
Applicant states that the present invention illustrates the detailed process of the present invention, but not office of the invention by above-described embodiment
It is limited to foregoing description, that is, does not mean that the present invention has to rely on foregoing detailed description and could implemented.The technology of art
Personnel it will be clearly understood that any improvement in the present invention, the addition of equivalence replacement and auxiliary element to each raw material of product of the present invention,
Selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (8)
1. a kind of preparation method of anode material for lithium-ion batteries, comprises the following steps：
(1) precursor of lithium ionic cell positive material powder is proportionally weighed, makes it well mixed；
(2) positive electrode material precursor after will be well mixed is suppressed；
(3) by the positive electrode material precursor both ends series connection access circuit after compacting, it is subsequently placed in incinerator, in the same of heating
When at positive electrode material precursor both ends apply 10V cm-1~400V cm-1Electric field, pass through when there is electric current in positive electrode material precursor
When, keeping temperature, by the Maximum constraint of current density in 10mA mm-2~1000mA mm-2, carry out electric current assisted with high-temperature conjunction
Into keeping the constant current density and heat preservation sintering certain time, obtaining anode material for lithium-ion batteries；Or
By in the positive electrode material precursor both ends series connection access circuit after compacting, it is subsequently placed in incinerator, is warming up to required temperature
Degree, then apply both ends to positive electrode material precursor and apply 10V cm-1~400V cm-1Electric field is until produce electric current, and by electricity
The Maximum constraint of current density is in 10mA mm-2~1000mA mm-2, electric current assisted with high-temperature synthesis is carried out, keeps the constant current
Density and heat preservation sintering certain time, obtain anode material for lithium-ion batteries.
A kind of 2. the method as described in claim 1, wherein the precursor of lithium ionic cell positive material includes lithium source and gold
Category source.
A kind of 3. method as claimed in claim 2, wherein the lithium source is compound or composition containing lithium.
A kind of 4. method as claimed in claim 3, wherein the compound or composition containing lithium are selected from lithium hydroxide, nitric acid
One in lithium, lithium carbonate, lithium oxalate, lithium fluoride, lithium bromide, lithium chloride, lithium acetate, lithia, lithium dihydrogen phosphate and lithium phosphate
Kind is a variety of.
A kind of 5. method as claimed in claim 3, wherein the compound or composition containing lithium are lithium hydroxide or carbonic acid
Lithium.
6. a kind of method as claimed in claim 2, wherein the source metal be selected from aluminium, magnesium, calcium, scandium, titanium, vanadium, chromium, manganese, iron,
Cobalt, nickel, copper, zinc, gallium, germanium, rubidium, strontium, yttrium, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, barium, hafnium, tantalum, tungsten,
Rhenium, osmium, iridium, platinum, gold, lanthanide series, the oxide of actinides, hydroxide, carbonate, oxalates, nitrate, fluoride
With the one or more in chloride.
A kind of 7. the method as described in claim 1, wherein the mode of the mixing is ball milling mixing, ground and mixed, ultrasound are mixed
Close or collosol and gel mixes.
8. a kind of the method as described in claim 1, wherein the positive electrode material precursor using sol-gal process, hydro-thermal method,
It is prepared by solid-phase synthesis, method of electrostatic spinning, microemulsion method or coprecipitation.
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Cited By (4)
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| CN109037672A (en) * | 2018-09-13 | 2018-12-18 | 广东邦普循环科技有限公司 | A kind of preparation method of power battery nickel-cobalt lithium manganate material |
| CN109056194A (en) * | 2018-07-12 | 2018-12-21 | 东华大学 | A kind of flexibility Li-La-Ti oxygen ceramic nanofibers membrane material and preparation method thereof |
| CN109608192A (en) * | 2018-12-29 | 2019-04-12 | 中原工学院 | A kind of method that electric field-assisted method prepares LLZO series battery material |
| CN109638276A (en) * | 2018-12-29 | 2019-04-16 | 中原工学院 | A kind of complete densification LLZO series solid state battery material and preparation method thereof |
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| CN109638276A (en) * | 2018-12-29 | 2019-04-16 | 中原工学院 | A kind of complete densification LLZO series solid state battery material and preparation method thereof |
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Application publication date: 20180119 |