CN106340634B - A kind of lithium titanate composite material and preparation method thereof - Google Patents
A kind of lithium titanate composite material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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Abstract
The invention belongs to battery material technical field, and in particular to a kind of lithium titanate composite material and preparation method thereof.The composite is synthesized by titanium source, lithium source, and by nano phase ag_2 o, petroleum coke is composite modified prepares.Resulting materials have higher specific discharge capacity under low range, high magnification and discharging at low temperature and high multiplying power, while material has excellent cycle performance.
Description
Technical field
The invention belongs to battery material technical field, and in particular to a kind of lithium titanate composite material and preparation method thereof.
Background technology
Lithium ion battery with its specific energy it is high, have extended cycle life, memory-less effect, pollute the spies such as small and self-discharge rate is small
A kind of point, it is considered to be preferable energy storage system.But, with production, growth in the living standard, to the property of lithium ion battery
Higher requirement can be it is also proposed.Traditional carbon negative pole material is not enough in terms of high magnification and high security, first
First, the current potential of Carbon anode and the current potential of lithium very close to, during over-charging of battery, lithium metal easily forms a tunic with electrolyte at interface,
And easily form Li dendrite；Secondly, graphite cathode due to layer structure, Lithium-ion embeding it is embedding go out process easily cause compared with large deformation
（10.3%）, cause cycle performance not enough；Finally, ion mobility of the lithium ion in graphite cathode is relatively low, causes charge and discharge
Electricity is slower, is not suitable for needing equipment of moment heavy current etc..Therefore need to find the more excellent alternative carbon material of performance
Novel anode material.And lithium titanate causes the extensive concern of people due to its unique performance.Although lithium titanate as lithium from
Sub- cell negative electrode material has many outstanding features, but lithium titanate also has its weak point, and such as high potential brings the low electricity of battery
Pressure, its intrinsic electrical conductivity is only 10-9S/cm, electron conduction is poor, and heavy-current discharge is also easy to produce larger polarization and specific capacity declines
Subtract very fast, this limits the multiplying power performance of the material to a certain extent.
In order to improve the performance of lithium titanate material, the widely used modified measures of current industrial quarters include：（1）It is miscellaneous
Atom is bulk phase-doped.It can be divided into according to the difference of doped chemical：It is cation doping, anion doped and composite mixed.Sun
Ion doping can make layer structure more complete, improve the stability of crystal structure, reduce Ni, Li mixing, reduce cyclic process
In capacity attenuation, this is obvious to the cycle performance and the effect of heat endurance that improve material.Anion doped master
If the doping F atom close with oxygen atom radius.Doping F can promote the sintering of material in appropriate amount, make the knot of positive electrode
Structure is more stablized, while the interface in cyclic process between stabilizing actives and electrolyte, improves the circulation of positive electrode
Performance and heat endurance；（2）Optimized production process.Production technology is improved, control prepares environment, humidity, atmosphere of material etc., than
Surface residual alkali content is such as reduced, particle diameter distribution uniformity is improved, improves Crystalline Quality, reduces the content segmented in material
Deng；（3）Surface coating, makes material separate to reduce material and electrolyte side reaction with electrolyte machinery, suppresses metal ion
Dissolving, reduce material repeated charge process in which materials structure the security caved in and then improve material.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, existing resource is made full use of, is postponed from from residual oil
There is provided a kind of lithium titanate composite material and preparation method thereof, resulting materials multiplying power as raw materials for production for the petroleum coke of coking
Performance, security performance are excellent, with higher charge/discharge capacity and higher cyclical stability.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of preparation method of lithium titanate composite material, comprises the following steps：
（1）With hydrogen peroxide and oxalic acid in mass ratio 1：2-3 constitutes composite detergent, composite detergent concentration of polymer solution
It is 1 in mass ratio by nano phase ag_2 o and compound washing agent solution for 15-35%:After 2-4 immersion nano phase ag_2 os 1-3h, mistake
Filter and washed with clear water, then dried at 100-120 DEG C, obtain the high-purity nm silver oxide that granularity is 10-25nm；
（2）By lithium source and titanium source compound, compare Li according to the amount of material：Ti=0.8~1.0：1 carries out dispensing, with anhydrous
Ethanol as solvent, compound concentration is 0.1-2mol/L lithium source solution respectively, and concentration is 0.1-2mol/L titanium source solution, weighs lithium source
With titanium source gross mass 1%-8% chelating agent, under ultrasonication, lithium source solution, titanium source solution are mixed, it is then slow to add
Enter chelating agent, continue ultrasound 2-4h, then the stirred in water bath 1-10h at 40 DEG C -80 DEG C, obtains gel；
（3）Petroleum coke is calcined purifying at 200-500 DEG C, the quality of high-energy ball milling, ball-milling medium and compound is carried out
Than for 5-10：1, rotating speed is 400-600r/min, ball milling 2-4h, is then dispersed in acid and carries out ultrasonically treated, finally leads to
Cross centrifugation, repeatedly washing and suction filtration product is reached neutrality, dry petroleum coke powder；
（4）It is 0.001-0.1 according to end-product petrochina is burnt with the mass ratio of lithium titanate under Ultrasonic Conditions：100
Ratio, petroleum coke powder is added to step（2）Gel in, gained gel is filtered, washed, dry, obtain presoma
Xerogel；
（5）By step（1）High-purity nm silver oxide add step（4）In described forerunner's xerogel, high energy ball is carried out
The mass ratio of mill, ball-milling medium and compound is 5-10：1, rotating speed is 400-600r/min, ball milling 2-4h, finally in indifferent gas
10~24h is sintered in 600 DEG C~800 DEG C under atmosphere, lithium titanate composite material is obtained after cooling.The particle diameter of ball-milling medium can be according to ball
Time consuming and the ball milling effect to be reached are selected, and the particle diameter of ball-milling medium preferably is 2-8mm.
Preferably, the lithium source is lithium nitrate.
Preferably, the titanium source is butyl titanate.
Preferably, the chelating agent is tartaric acid.
Preferably, in order to reduce cost, the recycling of petroleum coke, delay coke of the petroleum coke from residual oil are realized
The coke of change process formation.
Preferably, step（3）In acid be phosphoric acid.
A kind of lithium titanate composite material, is prepared according to above-mentioned preparation method.
The present invention has the advantages and positive effects of：
（1）Petroleum coke from residual oil delayed coking is used in the preparation of lithium titanate material, on the one hand solves oil
Jiao is difficult to the great difficult problem of recycling；On the other hand to giving full play to advantage of the petroleum coke in lithium titanate composite material,
Improving mortar construction quality and durability etc. has positive realistic meaning.In petroleum coke ash content essential element be iron, silicon, calcium,
Aluminium, sodium, magnesium, also a small amount of vanadium, titanium, chromium etc., it, which is doped in lithium titanate composite material, can make material in low range, high power
Rate under discharging at low temperature and high multiplying power with having higher specific discharge capacity, while the cycle performance of material can also be improved；
（2）Dopen Nano silver oxide, acts not only as the nucleator of lithium titanate, and obtained material particle size is nanometer
Level, uniform particle sizes, improve the electrical conductivity of material, the silver oxide of addition can also be conducive to electronics in material as inner conductor
Fast transferring in structure, together with the metallic element in petroleum coke, is realized to the composite mixed of lithium titanate material, in petroleum coke
There is the metal such as Group IIA metal and vanadium, chromium electron hole to supply Ion transfer there is provided sufficiently large passage, make electronics with lithium from
Sub preferably embedded in lithium titanate structure and abjection, so that the purpose for improving material electronicses and ionic conductivity is reached, and then
Improve reversible capacity and improve cycle performance.
（3）Because nano lithium titanate composite is affected by temperature seriously, interparticle contact resistance is anxious with temperature reduction
Play rise, may cause chemical property of the nano barium titanate lithium material under the conditions of low temperature high magnification to be severely impacted, this hair
Bright is lithium source from the lithium nitrate with oxidizing property, single-size spherical lithium titanate material can be made, and then have material
There are preferable high rate during charging-discharging and high specific capacity, be satisfied with the use requirement under the conditions of low temperature high magnification.
Embodiment
The present invention is specifically described and illustrated below by embodiment：
Embodiment 1
A kind of lithium titanate composite material, its preparation method is：（1）With hydrogen peroxide and oxalic acid in mass ratio 1：2 compositions are multiple
Detergent is closed, composite detergent concentration of polymer solution is 35%, is in mass ratio with compound washing agent solution by nano phase ag_2 o
1:After 2 immersion nano phase ag_2 o 3h, filter and washed with clear water, then dried at 100 DEG C, it is 10-25nm's to obtain granularity
High-purity nm silver oxide；
（2）By lithium source and titanium source compound, compare Li according to the amount of material：Ti=1.0：1 carries out dispensing, is made with absolute ethyl alcohol
Solvent, compound concentration is 0.1mol/L lithium source solution respectively, and concentration is 2mol/L titanium source solution, weighs lithium source and titanium source gross mass
1% chelating agent, under ultrasonication, lithium source solution, titanium source solution are mixed, then slow to add chelating agent, are continued
Ultrasonic 4h, then the stirred in water bath 10h at 40 DEG C, obtains gel；
（3）Petroleum coke is calcined purifying at 200 DEG C, high-energy ball milling is carried out, the mass ratio of ball-milling medium and compound is
10：1, rotating speed is 400r/min, ball milling 4h, be then dispersed in acid carry out it is ultrasonically treated, finally by centrifuge,
Washing and suction filtration make product reach neutrality repeatedly, dry petroleum coke powder；
（4）It is 0.001 according to end-product petrochina is burnt with the mass ratio of lithium titanate under Ultrasonic Conditions：100 ratio
Example, step is added to by petroleum coke powder（2）Gel in, gained gel is filtered, washed, dry, obtain forerunner's soma coagulate
Glue；
（5）By step（1）High-purity nm silver oxide add step（4）In described forerunner's xerogel, high energy ball is carried out
The mass ratio of mill, ball-milling medium and compound is 10：1, rotating speed is 400r/min, ball milling 4h, finally under an inert atmosphere in
600 DEG C of sintering 24h, lithium titanate composite material is obtained after cooling.
The lithium titanate composite material that the present embodiment is prepared is used as cell negative electrode material, and discharge capacity is up to 0.2C first
188mAh/g, 10C discharge capacity 112mAh/g, 2C discharge capacities are 121 mAh/g at 0 DEG C, after 1000 circulations of 2C multiplying powers
Capability retention is 96.4%.
Embodiment 2
A kind of lithium titanate composite material, its preparation method is：（1）With hydrogen peroxide and oxalic acid in mass ratio 1：3 compositions are multiple
Detergent is closed, composite detergent concentration of polymer solution is 15%, is in mass ratio with compound washing agent solution by nano phase ag_2 o
1:After 4 immersion nano phase ag_2 o 1h, filter and washed with clear water, then dried at 120 DEG C, obtain granularity for 10-25nm
High-purity nm silver oxide；
（2）By lithium source and titanium source compound, compare Li according to the amount of material：Ti=0.8：1 carries out dispensing, is made with absolute ethyl alcohol
Solvent, compound concentration is 2mol/L lithium source solution respectively, and concentration is 0.1mol/L titanium source solution, weighs lithium source and titanium source gross mass
8% chelating agent, under ultrasonication, lithium source solution, titanium source solution are mixed, then slow to add chelating agent, are continued
Ultrasonic 2h, then the stirred in water bath 1h at 80 DEG C, obtains gel；
（3）Petroleum coke is calcined purifying at 500 DEG C, high-energy ball milling is carried out, the mass ratio of ball-milling medium and compound is
5：1, rotating speed is 600r/min, ball milling 2h, be then dispersed in acid carry out it is ultrasonically treated, finally by centrifuging, anti-
Rehydration is washed makes product reach neutrality with suction filtration, dry petroleum coke powder；
（4）It is 0.1 according to end-product petrochina is burnt with the mass ratio of lithium titanate under Ultrasonic Conditions：100 ratio,
Petroleum coke powder is added to step（2）Gel in, gained gel is filtered, washed, dry, obtain presoma xerogel；
（5）By step（1）High-purity nm silver oxide add step（4）In described forerunner's xerogel, high energy ball is carried out
The mass ratio of mill, ball-milling medium and compound is 5：1, rotating speed is 600r/min, ball milling 2h, finally under an inert atmosphere in 800
DEG C sintering 10h, obtain lithium titanate composite material after cooling.
The lithium titanate composite material that the present embodiment is prepared is used as cell negative electrode material, and discharge capacity is up to 0.2C first
191mAh/g, 10C discharge capacity 109mAh/g, 2C discharge capacities are 125 mAh/g at 0 DEG C, after 1000 circulations of 2C multiplying powers
Capability retention is 95.7%.
Embodiment 3
A kind of lithium titanate composite material, its preparation method is：（1）With hydrogen peroxide and oxalic acid in mass ratio 1：3 compositions are multiple
Detergent is closed, composite detergent concentration of polymer solution is 25%, is in mass ratio with compound washing agent solution by nano phase ag_2 o
1:After 3 immersion nano phase ag_2 o 2h, filter and washed with clear water, then dried at 110 DEG C, it is 10-25nm's to obtain granularity
High-purity nm silver oxide；
（2）By lithium source and titanium source compound, compare Li according to the amount of material：Ti=0.9：1 carries out dispensing, is made with absolute ethyl alcohol
Solvent, compound concentration is 1.5mol/L lithium source solution respectively, and concentration is 1.5mol/L titanium source solution, weighs lithium source and the total matter of titanium source
The chelating agent of amount 6%, under ultrasonication, lithium source solution, titanium source solution are mixed, then slow to add chelating agent, after
Continuous ultrasound 3h, then the stirred in water bath 5h at 70 DEG C, obtains gel；
（3）Petroleum coke is calcined purifying at 380 DEG C, high-energy ball milling is carried out, the mass ratio of ball-milling medium and compound is
8：1, rotating speed is 500r/min, ball milling 3h, be then dispersed in acid carry out it is ultrasonically treated, finally by centrifuging, anti-
Rehydration is washed makes product reach neutrality with suction filtration, dry petroleum coke powder；
（4）It is 0.06 according to end-product petrochina is burnt with the mass ratio of lithium titanate under Ultrasonic Conditions：100 ratio
Example, step is added to by petroleum coke powder（2）Gel in, gained gel is filtered, washed, dry, obtain forerunner's soma coagulate
Glue；
（5）By step（1）High-purity nm silver oxide add step（4）In described forerunner's xerogel, high energy ball is carried out
The mass ratio of mill, ball-milling medium and compound is 8：1, rotating speed is 500r/min, ball milling 3h, finally under an inert atmosphere in 720
DEG C sintering 16h, obtain lithium titanate composite material after cooling.
The lithium titanate composite material that the present embodiment is prepared is used as cell negative electrode material, and discharge capacity is up to 0.2C first
198mAh/g, 10C discharge capacity 137mAh/g, 2C discharge capacities are 144 mAh/g at 0 DEG C, after 1000 circulations of 2C multiplying powers
Capability retention is 98.3%.
Comparative example 1
A kind of lithium titanate composite material, its preparation method and composition remove the relevant step of nano phase ag_2 o with reference to embodiment 3
Suddenly.
The lithium titanate composite material that the present embodiment is prepared is used as cell negative electrode material, and discharge capacity is 0.2C first
129mAh/g, 10C discharge capacity 91mAh/g, 2C discharge capacities are 103 mAh/g, the appearance after 100 circulations of 2C multiplying powers at 0 DEG C
It is 95.1% to measure conservation rate.
Comparative example 2
A kind of lithium titanate composite material, its preparation method and composition are with reference to embodiment 3, without petroleum coke, removal step
（3）And step（4）, by step（5）In " by step（1）High-purity nm silver oxide add step（4）Described forerunner's xerogel
In " replace with " by step（1）High-purity nm silver oxide add step（2）In described gel ".
The lithium titanate composite material that the present embodiment is prepared is used as cell negative electrode material, and discharge capacity is 0.2C first
125mAh/g, 10C discharge capacity 89mAh/g, 2C discharge capacities are 118mAh/g, the appearance after 1000 circulations of 2C multiplying powers at 0 DEG C
It is 94.6% to measure conservation rate.
By the lithium titanate composite material obtained by above-described embodiment and comparative example, using following methods test electrochemistry circulation
Performance：By composite, conductive agent and binding agent by mass percentage 94：1：5 mix their dissolvings in a solvent, and control is solid
Content is coated in copper foil current collector 50%, vacuum drying, obtained cathode pole piece；Then prepared by traditional maturation process
LiPF6/EC+DMC+EMC (the v/v=1 of tertiary cathode pole piece, 1mol/L:1:1) electrolyte, Celgard2400 barrier films, shell
18650 cylinder cells are assembled using conventional production process, the charge-discharge test of cylindrical battery is then carried out.
By the use of above-mentioned lithium titanate composite material as negative material, commercialization ternary electrode material is positive electrode, respectively
The both positive and negative polarity pole piece of battery is made, then above-mentioned both positive and negative polarity electrode slice and membrane winding are injected electrolyte, are assembled into battery core
Soft-package battery.Its cycle performance is tested, after 2C high rate charge-discharges 1000 times, battery capacity conservation rate is obtained.
The lithium titanate that the present invention is provided is can be seen that from the performance test results of above-described embodiment and comparative example resulting materials
Composite property more preferably, significantly improves the power-performance of battery, have under high magnification and low-rate discharge compared with
High discharge capacity, its discharging at low temperature and high multiplying power capacity is also significantly better than comparative example, and improves the cycle life of battery.This
Outside, the discharge capacity first of embodiment sample is up to more than 188mAh/g, higher than theoretical specific capacity.This is probably due to carbon material
With reproducibility, cause the oxygen of lithium titanate to lack at high temperature, part titanic is reduced to trivalent by carbon, drop its molal weight
It is low, thus it is shown that higher specific capacity.
Claims (5)
1. a kind of preparation method of lithium titanate composite material, it is characterised in that comprise the following steps：
（1）With hydrogen peroxide and oxalic acid in mass ratio 1：2-3 constitutes composite detergent, and composite detergent concentration of polymer solution is
15-35%, is 1 in mass ratio by nano phase ag_2 o and compound washing agent solution:After 2-4 immersion nano phase ag_2 os 1-3h, filtering
And washed with clear water, then dried at 100-120 DEG C, obtain the high-purity nm silver oxide that granularity is 10-25nm；
（2）By lithium source and titanium source compound, compare Li according to the amount of material：Ti=0.8~1.0：1 carries out dispensing, uses absolute ethyl alcohol
Make solvent, compound concentration is 0.1-2mol/L lithium source solution respectively, concentration is 0.1-2mol/L titanium source solution, weighs lithium source and titanium
Source gross mass 1%-8% chelating agent, under ultrasonication, lithium source solution, titanium source solution is mixed, are then slowly added into
Chelating agent, continues ultrasound 2-4h, then the stirred in water bath 1-10h at 40 DEG C -80 DEG C, obtains gel；
（3）Petroleum coke is calcined purifying at 200-500 DEG C, high-energy ball milling is carried out, the mass ratio of ball-milling medium and compound is
5-10：1, rotating speed is 400-600r/min, ball milling 2-4h, be then dispersed in acid carry out it is ultrasonically treated, finally by from
Heart separation, repeatedly washing and suction filtration make product reach neutrality, dry petroleum coke powder；
（4）It is 0.001-0.1 according to end-product petrochina is burnt with the mass ratio of lithium titanate under Ultrasonic Conditions：100 ratio
Example, step is added to by petroleum coke powder（2）Gel in, gained gel is filtered, washed, dry, obtain forerunner's soma
Gel；
（5）By step（1）High-purity nm silver oxide add step（4）In described forerunner's xerogel, high-energy ball milling, ball are carried out
The mass ratio of grinding media and compound is 5-10：1, rotating speed is 400-600r/min, ball milling 2-4h, under an inert atmosphere finally
10~24h is sintered in 600 DEG C~800 DEG C, lithium titanate composite material is obtained after cooling；Wherein, the lithium source is lithium nitrate, described
The coke of delayed coking formation of the petroleum coke from residual oil.
2. the preparation method of lithium titanate composite material according to claim 1, it is characterised in that the titanium source is metatitanic acid four
Butyl ester.
3. the preparation method of lithium titanate composite material according to claim 1, it is characterised in that the chelating agent is winestone
Acid.
4. the preparation method of lithium titanate composite material according to claim 1, it is characterised in that step（3）In acid be
Phosphoric acid.
5. a kind of lithium titanate composite material, it is characterised in that the preparation method according to claim any one of 1-4 is prepared into
Arrive.
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Effective date of registration: 20190102 Address after: 050000 401-7 Workshop Building No. 2, Fangyi Science Park Area A, Shijiazhuang High-tech Zone, Hebei Province Co-patentee after: Zhang Cui Patentee after: Zhao Shijiazhuang New Energy Technology Co. Ltd. Address before: 050000 No. 340 Cooperative Road, Xinhua District, Shijiazhuang City, Hebei Province Patentee before: Zhao Shijiazhuang New Energy Technology Co. Ltd. |