CN103050662A - Lithium titanate/copper composite lithium ion battery negative electrode material and preparation method thereof - Google Patents

Lithium titanate/copper composite lithium ion battery negative electrode material and preparation method thereof Download PDF

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CN103050662A
CN103050662A CN2012105804096A CN201210580409A CN103050662A CN 103050662 A CN103050662 A CN 103050662A CN 2012105804096 A CN2012105804096 A CN 2012105804096A CN 201210580409 A CN201210580409 A CN 201210580409A CN 103050662 A CN103050662 A CN 103050662A
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lithium
copper
source
ion battery
titanate
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刘洪江
程崇领
施利毅
薛鑫
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DONGGUAN-SHU INSTITUTE OF NANOTECHNOLOGY
University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention discloses a lithium titanate/copper composite lithium ion battery negative electrode material. The lithium titanate/copper composite lithium ion battery negative electrode material is characterized by being prepared from the following components: titanium source, lithium source and copper source; the copper is distributed into nanometer lithium titanate uniformly through in-situ synthesis; the copper accounts for 0.01 to 5 percent of the weight of the composite negative electrode material; and the lithium titanate accounts for 95 to 99.99 percent of the weight of the composite negative electrode material. The invention further discloses a preparation method for the lithium titanate/copper composite lithium ion battery negative electrode material. The copper is added into the lithium titanate material, so that the high-magnification charge/discharge performance of the negative electrode material is enhanced, the electrical conductivity of the negative electrode material is improved, and the requirement of the modern society on application of the lithium ion battery is met.

Description

A kind of lithium titanate/copper composite lithium ion battery cathode material and preparation method thereof
Technical field
The invention belongs to the electrochemical power source technical field of material, be specifically related to a kind of lithium titanate/copper compound lithium ion negative material and preparation method thereof.
Background technology
Along with the fast development of society, the problem of energy and environment becomes increasingly conspicuous, and seeks new clean energy resource and replaces petroleum resources to become more urgent.Electrokinetic cell has been subject to the attention of countries in the world as a kind of new cleaning fuel.Electrokinetic cell is the core component of the removable consuming devices such as electric motor car, electric tool, and pure electric automobile (EV) or mixed power electric car (HEV) take electrokinetic cell as main or auxiliary power source are one of main development directions of car industry.Simultaneously, country has accelerated the adjustment of energy resource structure, greatly develops the renewable secondary energy sources such as wind energy, solar energy.There are the shortcomings such as discontinuous and unstable in these energy, in use need supporting energy storage device.The development of new-energy automobile and extensive energy-storage system is for the lithium ion battery industry provides good opportunity to develop and more wide development space.Simultaneously, also the performance of lithium ion battery is had higher requirement.
Lithium titanate (Li with spinel structure 4Ti 5O 12) be considered to that one of negative material of application prospect is arranged most.In lithium ion embedding and subtractive process, the lithium titanate with spinel structure unit cell volume is substantially constant, thereby is called as " zero strain " material.Lithium titanate with spinel structure has following advantage as the cathode of lithium battery of a new generation: 1) spinelle Li 4Ti 5O 12Theoretical specific capacity is 175mAh/g, and actual specific capacity can reach 160-165mAh/g 2) spinelle Li 4Ti 5O 12Structure and physico-chemical property are stable, not with electrolyte reaction, good cycle.Because the stability of its structure becomes safety and extended-life lithium ion battery negative material; 3) spinelle Li 4Ti 5O 12Chemical diffusion coefficient at normal temperatures is 2 * 10 -8Cm 2/ s, than large 1 order of magnitude of carbon negative pole material, it is faster to discharge and recharge speed.These advantages of lithium titanate battery are conducive to it in the application in electric motor car and energy storage field.At present, the lithium-ion-power cell take lithium titanate as negative pole has become both at home and abroad the competitively focus of exploitation.
As lithium ion battery negative material, the intrinsic conductivity of lithium titanate is 10 -9S/cm belongs to typical insulator, poorly conductive, and heavy-current discharge performance is poor.Usually the preparation method plays a crucial role to the final performance of material, now preparation spinel type lithium titanate (Li commonly used 4Ti 5O 12) method high temperature solid phase synthesis, sol-gal process are arranged.The lithium titanate material high rate charge-discharge poor-performing of these two kinds of method preparations, energy consumption is large in the course of reaction.In view of this, it is less to be necessary to research and develop a kind of energy consumption, has the preparation method of the lithium titanate material of satisfactory electrical conductivity and large high rate performance.
Summary of the invention
The objective of the invention is for above-mentioned deficiency, a kind of lithium titanate/copper composite lithium ion battery cathode material and preparation method thereof is provided, by in lithium titanate material, adding copper, thereby improve the high rate charge-discharge performance of negative material, improve the conductivity of material, to satisfy modern society to the requirement of lithium ion battery applications.
The technical scheme that the present invention adopts for achieving the above object is:
A kind of lithium titanate/copper composite lithium ion battery cathode material, it is made by following component: titanium source, lithium source and Tong Yuan; By the even distribution of the compound realization copper of original position in nano lithium titanate, wherein copper shared part by weight in composite negative pole material is 0.01～5%, and lithium titanate shared part by weight in composite negative pole material is 95～99.99%.
Described titanium source is titanium sulfate, butyl titanate, isopropyl titanate, metatitanic acid, one or more in the amorphous titania.
Described lithium source is one or more in lithia, lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, the lithium nitrate.
Described copper source is one or more in cupric oxide, copper carbonate, Kocide SD, Schweinfurt green, cupric oxalate, copper chloride, copper nitrate, the copper sulphate.
A kind of preparation method according to above-mentioned lithium titanate/copper composite lithium ion battery cathode material is characterized in that it may further comprise the steps:
(1) measures the titanium source, add in the deionized water, make dispersion liquid A;
(2) measuring ratio with the described titanium of step (1) source amount of substance is 1: 1.0～1.2 lithium source, is scattered in the deionized water, makes dispersion liquid B;
(3) measure the copper source, the quality that makes institute's cupric is 0.01～5% of step (1) the titanium source of measuring and step (2) the lithium source gross mass of measuring;
(4) will pour in the pyroreaction still after solution A, solution B and the mixing of copper source, then place the baking oven of 120～200 ℃ of conditions to react 5～24 hours, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with deionized water or ethanol washing, drying obtains Li under 60～120 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(5) with the presoma of step (4) gained sintering 1～5h under nitrogen atmosphere, 400～1000 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
Mix in the described dispersion liquid A of step (4), dispersion liquid B and copper source, carries out under magnetic agitation, and continue to stir 30 minutes.
The invention has the beneficial effects as follows:
1, the present invention adopts is that hydrothermal synthesis method is processed with solid phase and combined, and the titanium source disperses to react under higher temperatures with the lithium source in water again, has realized other dispersion of molecular level, and being more evenly distributed of particle is so that the size of product can remain on nano-scale.Nano level lithium titanate material is realized ion-exchange simultaneously under the hydro-thermal dynamic environment, react more abundant, heat energy and kinetic energy are converted to the material internal energy, greatly shortened the processing time, improve productive rate, reduced energy resource consumption and cost, simplified process conditions, the raw material range of choice is wide, is easy in industrial enforcement.
2, the present invention's doped with Cu under hydrothermal condition has improved the uniformity of doping and the electric conductivity of material; Simultaneously owing to shortened heat treatment time, the material grains refinement, even structure is conducive to the migration of lithium ion and moves out.
3, doped with Cu of the present invention is utilized its high conductance, improves the conductivity of material, reduces the polarization of resistance and material, when improving significantly the lithium titanate conductance, has effectively improved charge-discharge performance and cycle performance.
Description of drawings
Fig. 1 is the X-ray diffractogram of the prepared material of the present invention;
Fig. 2 is the scanning electron microscope (SEM) photograph that the present invention prepares material;
Fig. 3 is embodiment 2 and the cycle performance curve of the prepared material of Comparative Examples under the 0.1C multiplying power;
Fig. 4 is the first charge-discharge curves of embodiment 2 prepared materials under the 0.1C multiplying power.
Embodiment
Embodiment 1: referring to Fig. 1 to Fig. 2, and the lithium titanate that present embodiment provides/copper composite lithium ion battery cathode material, it is made by following component: titanium source, lithium source and Tong Yuan; By the even distribution of the compound realization copper of original position in nano lithium titanate, wherein copper shared part by weight in composite negative pole material is 0.01～5%, and lithium titanate shared part by weight in composite negative pole material is 95～99.99%.
Described titanium source is titanium sulfate, butyl titanate, isopropyl titanate, metatitanic acid, one or more in the amorphous titania.
Described lithium source is one or more in lithia, lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, the lithium nitrate.
Described copper source is one or more in cupric oxide, copper carbonate, Kocide SD, Schweinfurt green, cupric oxalate, copper chloride, copper nitrate, the copper sulphate.
Preparation method according to above-mentioned lithium titanate/copper composite lithium ion battery cathode material is characterized in that it may further comprise the steps:
(1) measures the titanium source, add in the deionized water, make dispersion liquid A;
(2) measuring ratio with the described titanium of step (1) source amount of substance is 1: 1.0～1.2 lithium source, is scattered in the deionized water, makes dispersion liquid B;
(3) measure the copper source, the quality that makes institute's cupric is 0.01～5% of step (1) the titanium source of measuring and step (2) the lithium source gross mass of measuring;
(4) will pour in the pyroreaction still after dispersion liquid A, dispersion liquid B and the mixing of copper source, then place the baking oven of 120～200 ℃ of conditions to react 5～24 hours, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with deionized water or ethanol washing, drying obtains Li under 60～120 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(5) with the presoma of step (4) gained sintering 1～5h under nitrogen atmosphere, 400～1000 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
Mix in the described dispersion liquid A of step (4), dispersion liquid B and copper source, carries out under magnetic agitation, and continue to stir 30 minutes.
Embodiment 2: referring to Fig. 1 to Fig. 4, and the lithium titanate that present embodiment provides/copper composite lithium ion battery cathode material and preparation method thereof, substantially the same manner as Example 1, its difference is that it may further comprise the steps:
(1) measures the 28.46ml isopropyl titanate, splash in the 50ml deionized water, make dispersion liquid A;
(2) measure 4.2g hydronium(ion) oxidation lithium, with the ratio of the described isopropyl titanate amount of substance of step (1) be 1: 1, be scattered in the 50ml deionized water;
(3) measure the copper nitrate solution that 0.15ml concentration is 1mol/L, the quality that makes institute's cupric is 1 ‰ of isopropyl titanate and hydronium(ion) oxidation lithium gross mass, and copper nitrate solution is added in the dispersion liquid that step (2) makes, and makes dispersion liquid B;
(4) under magnetic agitation, the B dispersion liquid is slowly added in the A dispersion liquid, stir 30min, obtain reactant mixture;
(5) reactant mixture that step (4) is made is poured in the pyroreaction still, then places the baking oven of 160 ℃ of conditions to react 10h, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with the deionized water washing, drying obtains Li under 60 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(6) with the presoma of step (5) gained sintering 2h under nitrogen atmosphere, 500 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
Adopt the Rigaku D of company the max-2550X x ray diffractometer x to sample carry out material phase analysis (CuK α radiation, 40kV, 200mA, go on foot wide 0.02 °, 8 °/min of sweep speed, sweep limits (2 θ) is 10 °-70 °, such as Fig. 1; Adopt its pattern of S-4800 type sem observation, such as Fig. 2.
Be to mix at 80: 10: 10 according to active material, conductive carbon black, binding agent Kynoar (PVDF) mass ratio, film into the electrode film of the about 0.15mm of thickness with the wet film preparing device, 120 ℃ of dryings are 24 hours under vacuum, be cut into the electrode slice that diameter is 12mm with slicing machine, weigh and the accurate quality of calculated activity material.With metal lithium sheet as to electrode and reference electrode, Clegard2500 makes barrier film, the EC+DMC of 1mol/L LiPF6 (volume ratio 1: 1) solution is electrolyte (commerce is used electrolyte, has no special requirements), is assembled into 2016 type button cells in being full of the glove box of argon gas.On the LAND cell tester, carry out the test of cycle performance curve with the 0.1C multiplying power.
Cycle performance curve under 0.1C is seen Fig. 3, and first discharge specific capacity reaches 175mAhg-1.0.1C the specific capacity that discharges and recharges under the multiplying power after 100 weeks is 160mAhg-1, loses less.Fig. 4 is the prepared first charge-discharge platform curve of lithium titanate material under 0.1C, and its charge and discharge platform is obvious.
Embodiment 3: the lithium titanate that present embodiment provides/copper composite lithium ion battery cathode material and preparation method thereof, and with embodiment 1,2 basic identical, its difference is that it may further comprise the steps:
(1) measures the 10g amorphous titania, add in the 50ml deionized water, make dispersion liquid A;
(2) measure the 8.2g lithium nitrate, with the ratio of the described amorphous titania amount of substance of step (1) be 1: 1.05, be scattered in the 50ml deionized water;
(3) measure the copper-bath that 7.5ml concentration is 1mol/L, the quality that makes institute's cupric is 4% of amorphous titania and lithium nitrate gross mass, and copper-bath is added in the dispersion liquid that step (2) makes, and makes dispersion liquid B;
(4) under magnetic agitation, the B dispersion liquid is slowly added in the A dispersion liquid, stir 30min, obtain reactant mixture;
(5) reactant mixture that step (4) is made is poured in the pyroreaction still, then places the baking oven of 200 ℃ of conditions to react 10h, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with the deionized water washing, drying obtains Li under 60 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(6) with the presoma of step (5) gained sintering 5h under nitrogen atmosphere, 800 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
By the material of this method preparation, first discharge specific capacity reaches 170mAhg-1.0.1C the specific volume that discharges and recharges under the multiplying power after 100 weeks is 162mAhg-1, loses less.
Embodiment 4: the lithium titanate that present embodiment provides/copper composite lithium ion battery cathode material and preparation method thereof, and with embodiment 1,2,3 basic identical, its difference is that it may further comprise the steps:
(1) measures the 34ml butyl titanate, splash in the 100ml deionized water, make dispersion liquid A;
(2) measure the 9.27g lithium acetate, with the ratio of the described butyl titanate amount of substance of step (1) be 1: 1.1, be scattered in the 100ml deionized water, make dispersion liquid B;
(3) under magnetic agitation, the B dispersion liquid is slowly added in the A dispersion liquid, stir 30min, obtain reactant mixture;
(4) reactant mixture that step (3) is made is poured in the pyroreaction still, then places the baking oven of 160 ℃ of conditions to react 10h, and reaction naturally cools to room temperature after finishing, and then carries out suction filtration, and is with the deionized water washing, dry under 60 ℃ of conditions;
(5) get 0.5g step (4) gained material, and 0.05g CuSO 45H 2O adds in the 30ml deionized water, then joins in the reactor of 50ml, reacts 24h under 180 ℃ of conditions, then carries out suction filtration, and with the deionized water washing, 60 ℃ of dryings obtain Li 4Ti 5O 12/ Cu presoma;
(6) with the presoma of step (5) gained sintering 5h under nitrogen atmosphere, 650 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
Embodiment 5: the lithium titanate that present embodiment provides/copper composite lithium ion battery cathode material and preparation method thereof, and with embodiment 1,2,3,4 basic identical, its difference is that it may further comprise the steps:
(1) measures the 100g metatitanic acid, add in the 500ml deionized water, make dispersion liquid A;
(2) measure the 45.7g lithium chloride, with the ratio of the described metatitanic acid amount of substance of step (1) be 1: 1.15, be scattered in the 500ml deionized water;
(3) measure the copper chloride solution that 37.5ml concentration is 1mol/L, the quality that makes institute's cupric is 2% of metatitanic acid and lithium chloride gross mass, and copper chloride solution is added in the dispersion liquid that step (2) makes, and makes dispersion liquid B;
(4) under magnetic agitation, the B dispersion liquid is slowly added in the A dispersion liquid, stir 30min, obtain reactant mixture;
(5) reactant mixture that step (4) is made is poured in the pyroreaction still, then places the baking oven of 150 ℃ of conditions to react 24h, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with the deionized water washing, drying obtains Li under 60 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(6) with the presoma of step (5) gained sintering 5h under nitrogen atmosphere, 650 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
By the material of this method preparation, first discharge specific capacity reaches 174mAhg-1.0.1C the specific volume that discharges and recharges under the multiplying power after 100 weeks is 160mAhg-1, loses less.
Comparative Examples: present embodiment provides a kind of preparation method of pure lithium titanate anode material, and it may further comprise the steps:
(1) measures the 24ml isopropyl titanate, splash in the 500ml deionized water, make dispersion liquid A;
(2) measure 3.7g hydronium(ion) oxidation lithium, with the ratio of the described isopropyl titanate amount of substance of step (1) be 1: 1.1, be scattered in and make dispersion liquid B in the 500ml deionized water;
(3) under magnetic agitation, the B dispersion liquid is slowly added in the A dispersion liquid, stir 30min, obtain reactant mixture;
(4) reactant mixture that step (3) is made is poured in the pyroreaction still, then places the baking oven of 100 ℃ of conditions to react 10h, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with the deionized water washing, drying obtains Li under 60 ℃ of conditions 4Ti 5O 12Presoma;
(5) with the presoma of step (4) gained sintering 3h under nitrogen atmosphere, 800 ℃ of conditions, products therefrom namely gets pure lithium titanate material.
Above-mentioned pure lithium titanate material shows by contrast test, and its capacity is significantly less than the lithium titanate composite material that is mixed with copper that one's duty invention provides, and the specific capacity that has improved material of mixing of copper among the present invention is described, has improved the performance of material.
But the above only is better possible embodiments of the present invention, is not to limit to claim of the present invention, so the equivalent structure that all utilizations specification of the present invention and accompanying drawing content are done changes, all is included in protection scope of the present invention.

Claims (6)

1. lithium titanate/copper composite lithium ion battery cathode material is characterized in that it is made by following component: titanium source, lithium source and Tong Yuan; By the even distribution of the compound realization copper of original position in nano lithium titanate, wherein copper shared part by weight in composite negative pole material is 0.01～5%, and lithium titanate shared part by weight in composite negative pole material is 95～99.99%.
2. lithium titanate according to claim 1/copper composite lithium ion battery cathode material is characterized in that, described titanium source is titanium sulfate, butyl titanate, isopropyl titanate, metatitanic acid, one or more in the amorphous titania.
3. lithium titanate according to claim 1/copper composite lithium ion battery cathode material is characterized in that, described lithium source is one or more in lithia, lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium chloride, the lithium nitrate.
4. lithium titanate according to claim 1/copper composite lithium ion battery cathode material is characterized in that, described copper source is one or more in cupric oxide, copper carbonate, Kocide SD, Schweinfurt green, cupric oxalate, copper chloride, copper nitrate, the copper sulphate.
5. one kind according to claim 1 to the preparation method of one of 4 described lithium titanate/copper composite lithium ion battery cathode materials, it is characterized in that it may further comprise the steps:
(1) measures the titanium source, add in the deionized water, make dispersion liquid A;
(2) measuring ratio with the described titanium of step (1) source amount of substance is 1: 1.0～1.2 lithium source, is scattered in the deionized water, makes dispersion liquid B;
(3) measure the copper source, the quality that makes institute's cupric is 0.01～5% of step (1) the titanium source of measuring and step (2) the lithium source gross mass of measuring;
(4) will pour in the pyroreaction still after dispersion liquid A, dispersion liquid B and the mixing of copper source, then place the baking oven of 120～200 ℃ of conditions to react 5～24 hours, after reaction finishes, naturally cool to room temperature, then carry out suction filtration, with deionized water or ethanol washing, drying obtains Li under 60～120 ℃ of conditions 4Ti 5O 12/ Cu presoma;
(5) with the presoma of step (4) gained sintering 1～5h under nitrogen atmosphere, 400～1000 ℃ of conditions, products therefrom namely gets nanoscale Li 4Ti 5O 12/ Cu material.
6. the preparation method of described lithium titanate/copper composite lithium ion battery cathode material according to claim 5 is characterized in that, mix in the described dispersion liquid A of step (4), dispersion liquid B and copper source, carries out under magnetic agitation, and continues to stir 30 minutes.
CN2012105804096A 2012-12-27 2012-12-27 Lithium titanate/copper composite lithium ion battery negative electrode material and preparation method thereof Pending CN103050662A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140308200A1 (en) * 2013-04-12 2014-10-16 Hon Hai Precision Industry Co., Ltd. Method for making anode active material of lithium ion battery
CN104201344A (en) * 2014-09-05 2014-12-10 南开大学 Preparation method of copper-doped Li4Ti5O12-TiO2 regulation and control composite material
CN110518233A (en) * 2019-09-16 2019-11-29 广东工业大学 Graphite-doping lithium titanate anode material and preparation method thereof
CN110550654A (en) * 2019-09-16 2019-12-10 广东工业大学 Modified lithium titanate negative electrode material, preparation method thereof and battery
CN111244413A (en) * 2020-01-16 2020-06-05 河南工业大学 LTO/CVO composite material and preparation method thereof

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CN101986445A (en) * 2010-05-12 2011-03-16 罗劲松 Method for producing lithium battery cathode material lithium titanate
CN102610824A (en) * 2012-03-26 2012-07-25 上海大学 Preparation method of lithium titanate (Li4Ti5O12)/Ag composite lithium-ion negative electrode materials

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Publication number Priority date Publication date Assignee Title
CN101986445A (en) * 2010-05-12 2011-03-16 罗劲松 Method for producing lithium battery cathode material lithium titanate
CN102610824A (en) * 2012-03-26 2012-07-25 上海大学 Preparation method of lithium titanate (Li4Ti5O12)/Ag composite lithium-ion negative electrode materials

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140308200A1 (en) * 2013-04-12 2014-10-16 Hon Hai Precision Industry Co., Ltd. Method for making anode active material of lithium ion battery
US10106431B2 (en) * 2013-04-12 2018-10-23 Tsinghua University Method for making anode active material of lithium ion battery
CN104201344A (en) * 2014-09-05 2014-12-10 南开大学 Preparation method of copper-doped Li4Ti5O12-TiO2 regulation and control composite material
CN110518233A (en) * 2019-09-16 2019-11-29 广东工业大学 Graphite-doping lithium titanate anode material and preparation method thereof
CN110550654A (en) * 2019-09-16 2019-12-10 广东工业大学 Modified lithium titanate negative electrode material, preparation method thereof and battery
CN111244413A (en) * 2020-01-16 2020-06-05 河南工业大学 LTO/CVO composite material and preparation method thereof
CN111244413B (en) * 2020-01-16 2021-06-29 河南工业大学 LTO/CVO composite material and preparation method thereof

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Application publication date: 20130417