CN104934588A - Composite electrode material of lithium titanate surface load nanometer materials and preparation method and application thereof - Google Patents
Composite electrode material of lithium titanate surface load nanometer materials and preparation method and application thereof Download PDFInfo
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H—ELECTRICITY
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Abstract
The invention belongs to the technology field of lithium ion batteries and particularly relates to a composite electrode material of lithium titanate surface load nanometer materials and a preparation method and application thereof. On the basis of conventional lithium titanate, the composite electrode material is loaded with large-capacity novel negative electrode materials (metal oxides, metal elementary substances, metal alloy and the like). The composite electrode material has excellent cyclicity and high energy density, overcomes the defects that conventional lithium titanate materials are small in capacity, poor in multiplying power and difficulty in charge state detection and that metal elementary substances and metal oxides are poor in large-capacity negative cyclicity. Meanwhile, the composite electrode material has the advantages of easy charge state detection, large capacity, good cyclic performance and multiplying power property and is a novel negative electrode material for lithium ion batteries having promising application prospect on the basis of existing negative lithium titanate materials for lithium ion batteries.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to combination electrode material of a kind of lithium titanate load Large Copacity negative material of lithium ion battery and its preparation method and application.
Background technology
In recent years, day by day serious along with environmental problems such as the day by day exhausted of fossil energy and global warmings, the research that new forms of energy are correlated with has obtained social general attention.Come into the important step of productive life as new forms of energy, from the micro cell needed for compact electronic device to large electrical vehicular power source, lithium ion battery is just obtaining applying more and more widely.The thing followed, is also improving constantly the requirement of lithium ion battery, also imperative to the improvement of existing lithium ion battery.The improvement of performance of lithium ion battery depends primarily on the performance of the positive/negative doff lithium electrode material of battery.
With regard to the development of current lithium ion battery negative material, traditional carbon-based material successfully achieves business-like application, has in each side such as energy density, average working voltage, use voltage range, cycle life and self discharges the combination property being better than other rechargeable batteries.But the potential safety hazard that material with carbon element exists and not satisfactory cycle performance, impel people constantly to explore the substitute of carbon negative pole material.And compared to carbon based negative electrodes material, spinel type lithium titanate Li
4ti
5o
12material, in Lithium-ion embeding and the change in volume of deviating from recurring structure hardly in process, is called as " zero volume strain " material, therefore has the cycle life of overlength, and its higher charge and discharge platform (1.55 V
vs.li/Li
+), avoid the precipitation of Li dendrite and the formation of SEI film and the potential safety hazard of the battery short circuit caused, thus substantially increase the fail safe of battery.
As one business-like lithium ion battery negative material, the application of lithium titanate is very extensive.But in actual applications, due to its spinel structure, low electron conduction and ionic conductance, the impact of the intrinsic properties such as the electrode potential of Ti (IV)/Ti (III) oxidation-reduction pair, the further application of lithium titanate is faced with three large problems: due to each Li
4ti
5o
12three lithium ions only can be embedded in lattice, the energy density of lithium titanate anode material is relatively low, and (theoretical capacity is 175mAh/g only, the half of not enough graphite material theoretical energy density 372mAh/g, even lower than part anode material for lithium-ion batteries such as ternary materials), have a strong impact on the flying power of lithium ion battery.Because lithium titanate material electron conduction and ionic conductance are all lower, its high rate performance is poor, and during big current charge/discharge, capacitance loss is serious, limits the quick charge/discharge performance of lithium ion battery.Due to the restriction of Ti (IV)/Ti (III) oxidation-reduction pair itself, lithium titanate is at 1-3V(
vs.li/Li
+) between discharge curve present that bust-maintain an equal level-state of bust, this makes the Real-Time Monitoring of charge states of lithium ion battery (State of Charge, SOC) there is very large difficulty.If by the operating voltage interval extension of lithium titanate to 0-3V, its capacity can be increased to 250-300mAh/g, but its charge/discharge curve presents the state of bust-maintain an equal level-bust-fair, cannot improve the problem being difficult to detect SOC.Closely during the decade, based on metal oxide, metal simple-substance, the negative material of metal alloy etc. receives many concerns.As chrome green, tri-iron tetroxide, elemental silicon, signal bronze etc., these negative materials all have larger energy density, lower operating voltage (below 1V), and wherein portion of material, as tri-iron tetroxide, has good electron conduction.But the volumetric expansion in charge/discharge cycle process of these negative materials is very serious, easily causes the efflorescence of electrode material and comes off, having had a strong impact on the cycle performance of lithium ion battery.Generally speaking, this kind of electrode material 100 encloses the lower capability retention of circulation less than 10%.
Present invention employs a kind of is substrate with lithium titanate, the jumbo negative material of lithium titanate load.Utilize the advantage of lithium titanate " zero volume strain ", it can be used as the substrate of load, the Large Copacity negative material of nanometer is dispersed in the surface of lithium titanate material.This method for metal oxide equal-volume changes the cushion space that obvious negative material provides expansion, improves its cycle performance on the one hand.On the other hand, because the charge/discharge curve operating voltage of the Large Copacity negative materials such as metal oxide is in inclination to a certain degree, this composite material obviously can improve lithium titanate discharge platform smooth in discharge process.And because the conductivity of transition metal oxide or metal alloy compositions is better than lithium titanate, this composite material can improve the electron conduction of lithium titanate material effectively.
Instant invention overcomes traditional lithium titanate material capacity low, difference of magnification, the shortcomings such as state-of-charge detection difficult, propose a kind of Novel cathode material for lithium ion battery of lithium titanate loaded with nano Large Copacity negative material, can promote the chemical property of lithium titanate more all sidedly.
Summary of the invention
It is large that the object of the invention is to propose a kind of capacity, lithium ion battery combination electrode material of the lithium titanate loaded with nano negative material that multiplying power is high and preparation method thereof and application.
The lithium ion battery combination electrode material that the present invention proposes, is made up of the Large Copacity negative material of lithium titanate loaded with nano yardstick; Wherein, the lithium titanate as carrier comprises micro-meter scale lithium titanate, nanoscale lithium titanate (nanosphere, nano wire, mesoporous material, nano-micrometre ball) etc. a series of lithium titanate lithium ion battery negative material, its pattern comprises graininess, one-dimensional material, two-dimensional material etc.These materials have spinel structure, and chemical formula is Li
4ti
5o
12, Li
2ti
3o
7, or Type B TiO
2deng.The nanometer anode material of institute's load refers to that half-cell operating voltage is interval at 0-3V(
vs.li/Li
+) between, operating voltage is lower than the Large Copacity negative material of 1V.
In the present invention, described negative material comprises metal oxide and (includes but not limited to VO, V
2o
3, V
2o
5, Cr
2o
3, CrO
2, Cr
3o
4, CrO
3, FeO, Fe
3o
4, Fe
2o
3, CoO, Co
3o
4, NiO, Ni
2o
3, SnO, SnO
2and comprise the oxide etc. of multiple transition metal), metal simple-substance (includes but not limited to Sn, Al, Si), one or more the mixture such as metal alloy (including but not limited to kamash alloy, silicon-base alloy, germanium-base alloy, acieral, antimony-containing alloy, magnesium base alloy and other alloy).
In the present invention, the loading (carrying electrode materials quality/electrode material gross mass) between 5%-70% of the nano-electrode material of institute's load, if loading is less than 5%, then to lithium titanate capacity boost DeGrain, also not obvious on the impact of lithium titanate charge/discharge curve.If loading is greater than 70%, easily there is the reunion of nanometer anode material, seriously undermine the cycle performance of material.
In the present invention, described combination electrode material can adopt coprecipitation, hydro thermal method, sol-gal process, and local reduction way etc. obtain.
First kind coprecipitation, namely first by lithium titanate Li
4ti
5o
12by the methods such as stirring be scattered in solution containing one or more soluble metallic salts mutually in (water, ethanol etc. contribute to the solvent of dissolving metal salts), add precipitation reagent with vigorous stirring, control adds precipitation reagent quantity and concentration, obtains the Nanoscale metal oxide precipitation being deposited on lithium titanate surface.
Equations of The Second Kind hydro thermal method, lithium titanate is dispersed to solution mutually in, add the required reactant generating target product metal oxide/metal alloy/metal, and suitably regulate reactant ratio according to product chemistry formula.Gained suspension-turbid liquid liquid is loaded autoclave, the Large Copacity negative material of lithium titanate load can be obtained under the high temperature conditions.
3rd class sol-gal process, is scattered in lithium titanate in the solvent containing soluble metallic salt/soluble metal oxides, optionally adds a small amount of precipitation reagent, and solvent flashing is to obtain the composite material of lithium titanate load.
4th kind of local reduction way, for metal simple-substance, metal alloy etc., by the metal oxide of first obtained lithium titanate load, then by magnesiothermic reduction, Reduction of Oxide is metal simple-substance/metal alloy by the methods such as electrochemical reduction.
Large Copacity negative material described in this method, its yardstick is required to be nanoscale (between 1nm ~ 1 μm).If metal oxide-loaded, metal simple-substance, metal alloy granularity excessive, then the electrode material granules efflorescence caused by its volumetric expansion, come off and cannot overcome, the cyclicity of material will be subject to extreme influence.
Lithium titanate load Large Copacity negative material of the present invention can make the negative material of lithium ion battery.
Adopt the lithium ion battery that lithium titanate load Large Copacity negative material of the present invention and corresponding positive electrode are assembled, its energy density, multiplying power, the detection complexity of state-of-charge is all better than the lithium ion battery that traditional lithium titanate is assembled.
In the present invention, for assembling the positive electrode of lithium ion battery, be the LiM of spinel structure
2o
4the LiMO of layer structure
2, and the LiMPO of polyanion
4, Li
2mSiO
4(M is generally transition metal, comprises Mn, Co, Ni, Fe); And the material that other metallic elements Me of above-mentioned inlaid scheme adulterates, Me is one or more of Li, Mg, Cr, Al, Co, Ni, Mn, Al, Zn, Cu, La; Also comprise the part F of the compound of above-claimed cpd and doped with metal elements, the electrode material that S replaces.
Combination electrode material prepared by the present invention has excellent cyclicity and larger energy density, compensate for that traditional lithium titanate material capacity is too small, the deficiency of difference of magnification, state-of-charge detection difficult, also overcome the shortcoming that the Large Copacity such as metal simple-substance, metal oxide negative pole cyclicity is too poor simultaneously; The advantages such as also have simultaneously and be easy to state-of-charge detection, Large Copacity, cycle performance is good, and high rate performance is excellent, have the new negative electrode materials for lithium secondary batteries of good application prospect after being the existing lithium titanate anode material of a Similar integral.
Accompanying drawing explanation
Fig. 1 is the charge/discharge curve of lithium titanate load ferriferrous oxide composite material.
Fig. 2 is that the high rate performance curve of lithium titanate load ferriferrous oxide composite material compares with the high rate performance of pure lithium titanate.
Fig. 3 is the cycle performance curve of lithium titanate load ferriferrous oxide composite material.
Fig. 4 is the charge/discharge curve (source: G.-n. Zhu et al./Journal of Electroanalytical Chemistry, 688, (2013) 86 – 92) that the pure lithium titanate reported in document puts to 0V.
Fig. 5 is the charge/discharge curve of lithium titanate loaded with nano metal tin composite material.
Embodiment
Under by embodiment, the present invention is further illustrated.From following examples, the present invention may be better understood, but the present invention is not only confined to following examples.
Embodiment 1: take Iron(III) chloride hexahydrate (FeCl
36H
2o) 1.35g, is dissolved in 50mL ethylene glycol, obtains orange clear solution, then adds 3.6g sodium acetate (NaAc), stirs into yellow suspension, then takes 0.6g lithium titanate nano wire, joins in above-mentioned suspension-turbid liquid.Above-mentioned gained suspension-turbid liquid is added 200oC in autoclave and reacts 5 hours, by 80oC dried overnight after gained black product suction filtration.The loading of products therefrom and tri-iron tetroxide is about the lithium titanate load-type composite material of 70%.
Be that 9% Kynoar METHYLPYRROLIDONE solution fully grinds and becomes even pulpous state viscous fluid by above-mentioned made negative material powder and carbon black and concentration, wherein carbon black accounts for 10% of negative material powder weight, and Kynoar accounts for 10% of negative material powder weight.Then be coated with on Copper Foil, thickness is 0.1mm, carries out roll extrusion process after solvent evaporates under 1MPa pressure, to be placed in 80 ° of C vacuum drying ovens dry 12 hours afterwards, in this, as the work electrode of lithium ion battery.The test of row single electrode is put into according to the der group of positive pole/barrier film/negative pole in glove box.Single electrode test is with lithium sheet for negative pole, and 1M LiPF6 EC/DEC/DMC(volume ratio is 1:1:1) be electrolyte, barrier film adopts commercial li-ion battery diaphragm, is assembled into button cell (CR2016).Battery operated interval is 0 ~ 3.0V, and charging and discharging currents is 100mA/g, and recording its initial discharge capacity is 750mAh/g, second circle discharge capacity is 620mAh/g, after 100 circulations, capacity still maintains 600mAh/g, shows excellent cycle performance (Fig. 3).Compared with the charge/discharge curve (Fig. 4) of pure phase lithium titanate, this composite negative pole material not only shows the capacity of more than twice, and enclose from second, the obvious cancellation smooth charge/discharge platform of original existence, makes the detection simple and feasible more of the state-of-charge of the lithium ion battery assembled with this material.And due to the electron conduction that tri-iron tetroxide is excellent, the purer lithium titanate material of high rate performance of this composite material has had and has promoted significantly.
Embodiment 2: take Iron(III) chloride hexahydrate (FeCl
36H
2o) 1.35g, is dissolved in 50mL ethylene glycol, obtains orange clear solution, then adds 3.6g sodium acetate (NaAc), stirs into yellow suspension, then takes 1.2g lithium titanate nano wire, joins in above-mentioned suspension-turbid liquid.Above-mentioned gained suspension-turbid liquid is added 200oC in autoclave and reacts 5 hours, by 80oC dried overnight after gained black product suction filtration.The loading of products therefrom and tri-iron tetroxide is about the lithium titanate load-type composite material of 50%.
By above-mentioned made negative material powder according to method process, test in embodiment 1, find that this material initial discharge capacity is 580mAh/g, the second circle discharge capacity is 450mAh/g, and after 100 circle circulations, capacity dimension is held in 420mAh/g.This material also demonstrates the charge/discharge curve of relative canting.
Embodiment 3: take Iron(III) chloride hexahydrate (FeCl
36H
2o) 0.9g, is dissolved in 100mL water, takes green vitriol (FeSO
47H
2o) 0.9g, is dissolved in above-mentioned solution.Because divalent iron salt is in atmosphere than being easier to oxidation, therefore need to drop into excessive ferrous iron.Take 0.6g lithium titanate powder again, join in above-mentioned solution.Under agitation, instillation ammoniacal liquor (25%), continues stirring 2 hours.80oC dried overnight after gained black product is filtered.The loading of products therefrom and tri-iron tetroxide is about the lithium titanate load-type composite material of 70%.
By above-mentioned made negative material powder according to method process, test in embodiment 1, find that this material initial discharge capacity is 720mAh/g, the second circle discharge capacity is 570mAh/g, and after 100 circle circulations, capacity dimension is held in 500mAh/g.This material also demonstrates the charge/discharge curve of relative canting.
Embodiment 4: take Iron(III) chloride hexahydrate (FeCl
36H
2o) 1.35g, is dissolved in 50mL ethylene glycol, obtains orange clear solution, then adds 3.6g sodium acetate (NaAc), stirs into yellow suspension.Above-mentioned gained suspension-turbid liquid is added 200oC in autoclave and reacts 5 hours, by 80oC dried overnight after gained black product suction filtration, obtain ferriferrous oxide nano sphere.By gained ferriferrous oxide nano sphere according to mass ratio 7:3 with lithium titanate ground and mixed, make test negative pole.
By above-mentioned made negative material powder according to method process, test in embodiment 1.Recording this mixing negative pole initial discharge capacity is 800mAh/g, and the second circle discharge capacity is 540mAh/g, and after 100 circle circulations, the capacity of this material is only 125mAh/g, and demonstrates very large polarization.Because of when synthesizing the tri-iron tetroxide negative material of lithium titanate load, lithium titanate have the dispersion helping tri-iron tetroxide, obtain the ferriferrous oxide nano-particle that particle diameter is less, and in this embodiment, nano ferriferrous oxide not only particle diameter is larger, and there is no pay(useful) load on lithium titanate, the efflorescence of material, come off serious.Cause the cyclicity decay of negative pole serious.
Embodiment 5: take Chromium nitrate (Cr(NO3)3),nonahydrate (Cr (NO
3)
39H
2o) 1.2g was dissolved in the water, and adds the citric acid of equimolar amounts, adds 0.3g lithium titanate after dissolving, and in 70oC water-bath, complexing ageing is to the thick shape of glue, by this jelly 110oC drying 16 hours.Gained solid is calcined 8 hours under 650oC, obtains the negative material of lithium titanate load chrome green.
By above-mentioned made negative material powder according to method process, test in embodiment 1, find that this material initial discharge capacity is 800mAh/g, the second circle discharge capacity is 640mAh/g, and after 100 circle circulations, capacity dimension is held in about 610mAh/g.This material also demonstrates the charge/discharge curve of relative canting.
Embodiment 6: take two hydration stannous chloride (SnCl
22H
2o) 0.6g is dissolved in 90oC triethylene glycol/PVP solution under argon shield, adds 0.3g lithium titanate, stirs 30min again after stirring.And then add 25ml NaBH
4triethylene glycol suspension-turbid liquid (0.06g/mL), continue stir 30min.By product suction filtration, dry 6 hours of 80oC, obtains the negative material of lithium titanate loaded with nano metal tin.
By above-mentioned made negative material powder according to method process, test in embodiment 1, find that this material initial discharge capacity is 750mAh/g, the second circle discharge capacity is 430mAh/g, and after 100 circle circulations, capacity dimension is held in about 360mAh/g.This material also demonstrates the charge/discharge curve of canting.
Claims (8)
1. a combination electrode material for lithium titanate surface loaded with nano material, is characterized in that being made up of the Large Copacity negative material of lithium titanate loaded with nano yardstick; Wherein, the lithium titanate as carrier comprises micro-meter scale lithium titanate and nanoscale lithium titanate; The nanometer anode material of institute's load is that half-cell operating voltage is interval at 0-3V(
vs.li/Li
+) between, operating voltage is lower than the Large Copacity negative material of 1V.
2. combination electrode material according to claim 1, it is characterized in that the described lithium titanate as carrier has spinel structure, chemical formula is Li
4ti
5o
12, Li
2ti
3o
7, or Type B TiO
2.
3. combination electrode material according to claim 1, is characterized in that described nanometer anode material is selected from and comprises metal oxide, metal simple-substance, one or more mixture in metal alloy; Wherein, described metal oxide is VO, V
2o
3, V
2o
5, Cr
2o
3, CrO
2, Cr
3o
4, CrO
3, FeO, Fe
3o
4, Fe
2o
3, CoO, Co
3o
4, NiO, Ni
2o
3, SnO or SnO
2, described metal simple-substance is Sn, Al or Si, and described metal alloy is kamash alloy, silicon-base alloy, germanium-base alloy, acieral, antimony-containing alloy, magnesium base alloy or other alloy.
4., according to the combination electrode material one of claim 1-3 Suo Shu, it is characterized in that the load capacity of the Large Copacity negative material of described lithium titanate loaded with nano yardstick and the negative material quality of institute's load are 5%-70% with the ratio of gross mass.
5. the preparation method of combination electrode material as described in one of claim 1-4, is characterized in that the one adopting following method: coprecipitation, hydro thermal method, sol-gal process, local reduction way.
6. preparing the application in lithium ion battery by the described combination electrode material of one of claim 1-4 for one kind.
7. the lithium ion battery assembled as negative pole and corresponding positive electrode by the described combination electrode material of one of claim 1-4.
8. lithium ion battery according to claim 7, is characterized in that described positive electrode is: the LiM of spinel structure
2o
4, the LiMO of layer structure
2, or the LiMPO of polyanion
4or Li
2mSiO
4, M is transition metal: Mn, Co, Ni, or Fe; Or for above-mentioned inlaid scheme adulterates the material of other metallic elements Me, Me is one or more of Li, Mg, Cr, Al, Co, Ni, Mn, Al, Zn, Cu, La; Or be the electrode material that the part F of the compound of above-claimed cpd and doped with metal elements, S replace.
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| CN108187606A (en) * | 2018-01-22 | 2018-06-22 | 天津市职业大学 | A kind of electric conductivity titanium based lithium-ion sieve and preparation method thereof |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN110518233A (en) * | 2019-09-16 | 2019-11-29 | 广东工业大学 | Graphite-doping lithium titanate anode material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107768658A (en) * | 2017-11-16 | 2018-03-06 | 中南大学 | A kind of composite cathode material for lithium ion cell and preparation method thereof |
| CN107768658B (en) * | 2017-11-16 | 2020-03-06 | 中南大学 | Lithium ion battery composite negative electrode material and preparation method thereof |
| CN108187606A (en) * | 2018-01-22 | 2018-06-22 | 天津市职业大学 | A kind of electric conductivity titanium based lithium-ion sieve and preparation method thereof |
| CN108187606B (en) * | 2018-01-22 | 2020-07-17 | 天津市职业大学 | Conductive titanium lithium ion sieve and preparation method thereof |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN110518233A (en) * | 2019-09-16 | 2019-11-29 | 广东工业大学 | Graphite-doping lithium titanate anode material and preparation method thereof |
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Application publication date: 20150923 |