CN106910879A - In-situ preparation lithium titanate-composite titania material and preparation method thereof - Google Patents
In-situ preparation lithium titanate-composite titania material and preparation method thereof Download PDFInfo
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- CN106910879A CN106910879A CN201710195015.1A CN201710195015A CN106910879A CN 106910879 A CN106910879 A CN 106910879A CN 201710195015 A CN201710195015 A CN 201710195015A CN 106910879 A CN106910879 A CN 106910879A
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- 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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Abstract
The invention discloses a kind of in-situ preparation lithium titanate-composite titania material and preparation method thereof, the lithium titanate-composite titania material is divided into three layers from inside to outside, and innermost layer is lithium titanate, intermediate layer is titanium dioxide, and outermost layer is carbon.Its preparation method is comprised the following steps：Titanium dioxide is added in sodium hydrate aqueous solution carries out hydro-thermal reaction；Then product is added in acid solution, ion exchange is carried out, after centrifugation, solid adds lithium hydroxide solution, is well mixed, add hydrothermal reaction kettle reaction；This centrifugation, collected solid is once calcined again, obtains lithium titanate, adds organic carbon source ball milling, after baking to obtain the in-situ preparation lithium titanate-composite titania material.Lithium titanate-the composite titania material has core shell structure, can not only suppress product flatulence, moreover it is possible to product is had good security performance and structural stability can.
Description
Technical field
The present invention relates to ion secondary battery cathode material lithium field, more particularly to a kind of in-situ preparation lithium titanate-dioxy
Change titanium composite material and preparation method thereof.
Background technology
New lithium titanate material-Li4Ti5O12With larger lithium ion solid-state diffusion constant and sub-micron (or nanometer)
Particle diameter distribution, with excellent rapid charge characteristic (5 minutes full capacitances of charging capacity >=80%) and repid discharge performance is (most
50C can be carried out greatlyAMultiplying power discharging)；Lithium titanate anode does not produce lithium metal in charge and discharge process, simultaneously because lithium titanate anode
With excellent fast charging and discharging performance, thus electro-hydraulic with new high-viscosity noninflammability can use cooperatively, battery pack can hold
By 240 DEG C of high temperature impact, with high security performance；Lithium titanate material has the spinel structure of stabilization, in discharge and recharge
Process Volume Changes it is smaller (<0.2%), therefore with good cycle life, 1000 circulation volumes of high rate charge-discharge are protected
Holdup still can reach more than 90%.Lithium titanate anode, should in high power type lithium ion electrokinetic cell compared with traditional Li-C negative poles
Use with advantage, but the theoretical capacity of lithium titanate is only 175mAh/g, and it is have impact on to a certain extent in high-energy-density
Application on lithium-ion-power cell；The theoretical specific capacity of anatase titanium dioxide is up to 335mAh/g, and anatase titanium dioxide titanium dioxide
The presence of titanium can effectively improve the high rate performance of lithium titanate.Therefore, lithium titanate-composite titania material is up-and-coming
A kind of composite.But the carbonate solvent in electrolyte can be caused to decompose due to the presence of Ti-O keys, produce flatulence, have impact on
Its practical application.
The preparation method of common lithium titanate-composite titania material is：Lithium source and titanium source are added during the course of the reaction, its
The mol ratio of middle elemental lithium and titanium elements less than the stoichiometric proportion in lithium titanate, due to the presence of excessive Ti, generation lithium titanate-
Composite titania material, in composition lithium titanate and titanium dioxide mutually mix, the defect of the method is the mixing of lithium titanate
Uniformity is poor, and the presence of excess Ti easily generates other impurities compound, influences properties of product.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of in-situ preparation lithium titanate-composite titania material
And preparation method thereof, the lithium titanate-composite titania material has nucleocapsid structure, and coated by titanium dioxide is in the outer of lithium titanate
Surface, outermost layer cladding carbon-coating；Product flatulence can not only be suppressed, moreover it is possible to make product that there is good security performance and Stability Analysis of Structures
Performance.
Therefore, technical scheme is as follows：
A kind of in-situ preparation lithium titanate-composite titania material, is divided into three layers from inside to outside, innermost layer be lithium titanate,
Intermediate layer is titanium dioxide, and outermost layer is carbon.
It is preferred that, lithium titanate thickness degree is micron order, titanium dioxide layer thickness is submicron order, and carbon layers having thicknesses are nanoscale.
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, comprises the following steps：
1) titanium dioxide is added in sodium hydrate aqueous solution, is incubated in hydrothermal reaction kettle, at 180~210 DEG C anti-
18~48h is answered, material I is obtained；
Wherein the mol ratio of titanium dioxide and NaOH is 1：(6~24)；
2) the material I is added to 0.4~0.8mol/L [H+] acid solution in, described in wherein 1g material I correspondence plus
Enter acid solution described in 100~200ml, the reaction time is 12~48h, obtains ion exchange solution I；
3) the ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1~2mol/l, hydrothermal reaction kettle is added after being well mixed,
12~24h is incubated at 150~200 DEG C, ion exchange solution II is obtained；
5) the ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) the material III is once calcined at 750~800 DEG C, roasting time is 8~24h, obtains lithium titanate
Material；
7) by ball milling in the lithium titanate material, organic carbon source and deionized water addition sand mill, material IV is obtained；It is described
The quality of organic carbon source is the 5~10% of lithium titanate material quality；
8) the material IV is spray-dried, drying temperature is 240~280 DEG C, obtains material V；
9) the material V is carried out into after baking under inert gas shielding atmosphere, sintering temperature is 750~850 DEG C, roasting
The burning time is 6~12h, that is, obtain the in-situ preparation lithium titanate-composite titania material.
Further, step 2) acid solution be hydrochloric acid or sulfuric acid.
Further, step 7) organic carbon source be phenolic resin or polyvinylpyrrolidone.
Further, step 9) inert gas be nitrogen, helium and argon gas.
A kind of in-situ preparation lithium titanate-composite titania material of present invention offer and preparation method thereof, the lithium titanate-
Composite titania material be structurally characterized in that two layers cladding nucleocapsid structures；Wherein outermost layer be carbon, intermediate layer be titanium dioxide
Titanium, innermost layer are lithium titanate.Carbon-coating ensure that composite has good electric conductivity, and titanium dioxide layer ensure that composite
With specific capacity higher, metatitanic acid lithium layer ensure that material has good security performance and structural stability can.The preparation side
Method generates pure phase lithium titanate material first with two one-step hydrothermals, and the carbon source and lithium titanate for secondly adding cladding occur high temperature solid-state
Reaction；The effect of carbon source mainly has following three points：1. composite electron conduction is improved, 2. suppresses composite flatulence, 3.
Meeting generating portion lithia steam during carbon coating, makes lithium titanate top layer that exploded, generation titanium dioxide/titanium acid lithium occur
Nucleocapsid structure.
Brief description of the drawings
The structural representation of in-situ preparation lithium titanate-composite titania material that Fig. 1 is provided for the present invention；
Fig. 2 is thing phase (XRD) figure of in-situ preparation lithium titanate-composite titania material obtained in embodiment 1.
Specific embodiment
Technical scheme is described in detail below in conjunction with accompanying drawing.
Embodiment 1
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, comprises the following steps：
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is incubated at 180 DEG C
48h, obtains material I；
Wherein the mol ratio of titanium dioxide and NaOH is 1:6；
2) material I is added to 0.4mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solutions=1g/200ml, instead
It is 48h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1mol/l, hydrothermal reaction kettle is added after being well mixed, at 150 DEG C
Lower insulation 24h, obtains ion exchange solution II；
5) ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) material III is once calcined at 750 DEG C, roasting time is 24h, obtains lithium titanate material；
7) by ball milling in lithium titanate material, phenolic resin and deionized water addition sand mill, the quality of phenolic resin is titanium
The 5% of sour lithium material quality；Obtain material IV；
8) material IV is spray-dried, drying temperature is 280 DEG C, obtains material V；
9) material V is carried out into after baking under nitrogen atmosphere, sintering temperature is 750 DEG C, and roasting time is 12h, is obtained final product
To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because after baking shape
Into titanium dioxide layer.
Embodiment 2
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, comprises the following steps：
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is incubated at 210 DEG C
18h, obtains material I；
Wherein the mol ratio of titanium dioxide and NaOH is 1:12；
2) material I is added to 0.8mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solutions=1g/100ml, instead
It is 12h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after being well mixed, at 200 DEG C
Lower insulation 12h, obtains ion exchange solution II；
5) ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) material III is once calcined at 800 DEG C, roasting time is 8h, obtains lithium titanate material；
7) by ball milling, polyvinylpyrrolidine in lithium titanate material, polyvinylpyrrolidone and deionized water addition sand mill
The quality of ketone is the 7% of lithium titanate material quality, obtains material IV；
8) material IV is spray-dried, drying temperature is 280 DEG C, obtains material V；
9) material V is carried out into after baking under helium atmosphere, sintering temperature is 800 DEG C, and roasting time is 10h, is obtained final product
To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because after baking shape
Into titanium dioxide layer.
Embodiment 3
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is incubated at 200 DEG C
36h, obtains material I；
Wherein the mol ratio of titanium dioxide and NaOH is 1:18；
2) material I is added to 0.8mol/L [H+] sulfuric acid solution in, wherein material I/ acid solutions=1g/150ml, instead
It is 36h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after being well mixed, at 180 DEG C
Lower insulation 18h, obtains ion exchange solution II；
5) ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) material III is once calcined at 800 DEG C, roasting time is 12h, obtains lithium titanate material；
7) by ball milling, polyvinylpyrrolidine in lithium titanate material, polyvinylpyrrolidone and deionized water addition sand mill
The quality of ketone is the 10% of lithium titanate material quality, obtains material IV；
8) material IV is spray-dried, drying temperature is 260 DEG C, obtains material V；
9) material V is carried out into after baking under argon atmosphere, sintering temperature is 800 DEG C, and roasting time is 10h, is obtained final product
To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because after baking shape
Into titanium dioxide layer.
Embodiment 4
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, comprises the following steps：
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is incubated at 200 DEG C
48h, obtains material I；
Wherein the mol ratio of titanium dioxide and NaOH is 1:24；
2) material I is added to 0.8mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solutions=1g/200ml, instead
It is 24h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after being well mixed, at 180 DEG C
Lower insulation 24h, obtains ion exchange solution II；
5) ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) material III is once calcined at 750 DEG C, roasting time is 24h, obtains lithium titanate material；
7) by ball milling in lithium titanate material, phenolic resin and deionized water addition sand mill, the quality of phenolic resin is titanium
The 9% of sour lithium material quality, obtains material IV；
8) material IV is spray-dried, drying temperature is 260 DEG C, obtains material V；
9) material V is carried out into after baking under nitrogen atmosphere, sintering temperature is 800 DEG C, and roasting time is 12h, is obtained final product
To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because after baking shape
Into titanium dioxide layer.
Experimental conditions：
Fig. 1 is the structural representation of the obtained in-situ preparation lithium titanate-composite titania material of the present invention；Can by figure
See, outermost layer 1 is cladding carbon material, intermediate layer 2 is the anatase titanium dioxide being formed in situ, and innermost layer 3 is spinelle metatitanic acid
Lithium.The structure can ensure that product of the present invention has specific capacity higher compared with pure phase lithium titanate, and can effectively suppress bulging
It is swollen.
Table 1 is listed and is made button cell first using ion secondary battery cathode material lithium obtained in above-described embodiment
Cycle charge discharge capacitance and actual effect cycle performance of battery.The test condition of button cell be LR 2032,0.1C, 1.0~3.0V,
vs.Li+/Li；The test condition of actual effect battery is that ICP053048,5C, 2.0~2.9V, the charging/discharging apparatus for using are electric for orchid
Discharge and recharge instrument.
The cycle performance of table 2 tests table
The lithium titanate anode material cycle performance that can be seen that present invention preparation by data in table is fine, after 1000 weeks
Not there is bulging phenomenon still more than 100%, and due to the effect of carbon coating in capability retention.
Fig. 2 is thing phase (XRD) figure of in-situ preparation lithium titanate-composite titania material obtained in example 2, can by figure
To find out the composite for preparing based on lithium titanate, with the presence of a small amount of anatase titanium dioxide, because carbon is amorphous
State and content is relatively low, therefore exist without carbon peak.
Claims (6)
1. a kind of in-situ preparation lithium titanate-composite titania material, it is characterised in that：It is divided into three layers, innermost layer from inside to outside
For lithium titanate, intermediate layer are titanium dioxide, outermost layer is carbon.
2. in-situ preparation lithium titanate-composite titania material as claimed in claim 1, it is characterised in that：Lithium titanate thickness degree
For micron order, titanium dioxide layer thickness are submicron order, carbon layers having thicknesses are nanoscale.
3. a kind of preparation method of in-situ preparation lithium titanate-composite titania material, it is characterised in that comprise the following steps：
1) titanium dioxide is added in sodium hydrate aqueous solution, in hydrothermal reaction kettle, insulation reaction 18 at 180~210 DEG C
~48h, obtains material I；
Wherein the mol ratio of titanium dioxide and NaOH is 1：6~24；
2) the material I is added to 0.4~0.8mol/L [H+] acid solution in, described in wherein 1g material I correspondence add 100
Acid solution described in~200ml, the reaction time is 12~48h, obtains ion exchange solution I；
3) the ion exchange solution I is put into be washed in supercentrifuge and is separated, collect solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1~2mol/l, it is well mixed after add hydrothermal reaction kettle, 150~
12~24h is incubated at 200 DEG C, ion exchange solution II is obtained；
5) the ion exchange solution II is washed into separation in supercentrifuge, collects solid, obtain material III；
6) the material III is once calcined at 750~800 DEG C, roasting time is 8~24h, obtains lithium titanate material
Material；
7) by ball milling in the lithium titanate material, organic carbon source and deionized water addition sand mill, material IV is obtained；It is described organic
The quality of carbon source is the 5~10% of lithium titanate material quality；
8) the material IV is spray-dried, drying temperature is 240~280 DEG C, obtains material V；
9) the material V is carried out into after baking under inert gas shielding atmosphere, sintering temperature is 750~850 DEG C, during roasting
Between be 6~12h, that is, obtain the in-situ preparation lithium titanate-composite titania material.
4. the preparation method of in-situ preparation lithium titanate-composite titania material as claimed in claim 3, it is characterised in that：Step
Rapid 2) described acid solution is hydrochloric acid or sulfuric acid.
5. the preparation method of in-situ preparation lithium titanate-composite titania material as claimed in claim 3, it is characterised in that：Step
Rapid 7) described organic carbon source is phenolic resin or polyvinylpyrrolidone.
6. the preparation method of in-situ preparation lithium titanate-composite titania material as claimed in claim 3, it is characterised in that：Step
Rapid 9) described inert gas is nitrogen, helium and argon gas.
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Cited By (2)
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| CN107808953A (en) * | 2017-10-17 | 2018-03-16 | 合肥国轩高科动力能源有限公司 | A kind of preparation method for the lithium titanate anode material that moisture absorption is low, aerogenesis is few |
| CN111129441A (en) * | 2018-10-30 | 2020-05-08 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material and preparation method thereof, lithium ion battery cathode and lithium ion battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107808953A (en) * | 2017-10-17 | 2018-03-16 | 合肥国轩高科动力能源有限公司 | A kind of preparation method for the lithium titanate anode material that moisture absorption is low, aerogenesis is few |
| CN107808953B (en) * | 2017-10-17 | 2020-05-22 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium titanate negative electrode material with low moisture absorption and less gas generation |
| CN111129441A (en) * | 2018-10-30 | 2020-05-08 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material and preparation method thereof, lithium ion battery cathode and lithium ion battery |
| CN111129441B (en) * | 2018-10-30 | 2021-06-18 | 深圳市比亚迪锂电池有限公司 | Lithium ion battery cathode material, preparation method thereof, cathode and lithium ion battery |
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