CN106910879B - 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 PDF

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CN106910879B
CN106910879B CN201710195015.1A CN201710195015A CN106910879B CN 106910879 B CN106910879 B CN 106910879B CN 201710195015 A CN201710195015 A CN 201710195015A CN 106910879 B CN106910879 B CN 106910879B
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lithium titanate
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composite titania
titanium dioxide
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CN106910879A (en
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宋英杰
徐宁
伏萍萍
马倩倩
吴孟涛
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Tianjin B&M Science and Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
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  • Composite Materials (AREA)
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  • Manufacturing & Machinery (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of in-situ preparation lithium titanate-composite titania material and preparation method thereof, which is divided into three layers from inside to outside, and innermost layer is lithium titanate, middle layer is titanium dioxide, and outermost layer is carbon.Preparation method includes the following steps: titanium dioxide being added in sodium hydrate aqueous solution and carries out hydro-thermal reaction；Then product is added in acid solution, carries out ion exchange, after centrifugation, lithium hydroxide solution is added in solid, is uniformly mixed, and hydrothermal reaction kettle reaction is added；This is centrifuged again, and collected solid is once roasted, and obtains lithium titanate, and organic carbon source ball milling is added, and after baking obtains the in-situ preparation lithium titanate-composite titania material.Lithium titanate-the composite titania material has nucleocapsid structure, can not only inhibit product flatulence, moreover it is possible to product be made to have good security performance and structural stability can.

Description

In-situ preparation lithium titanate-composite titania material and preparation method thereof
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-dioxies Change titanium composite material and preparation method thereof.
Background technique
Novel lithium titanate material-Li4Ti5O12With biggish lithium ion solid-state diffusion constant and sub-micron (or nanometer) Particle diameter distribution has excellent rapid charge characteristic (charging capacity >=80% expired capacitance in 5 minutes) and repid discharge performance is (most 50C can be carried out greatlyAMultiplying power discharging)；Lithium titanate anode does not generate lithium metal in charge and discharge process, simultaneously because lithium titanate anode With excellent fast charging and discharging performance, thus can with novel highly viscous noninflammability is electro-hydraulic is used cooperatively, battery pack can be held By 240 DEG C of high temperature impact, there is high security performance；Lithium titanate material has stable spinel structure, in charge and discharge Process volume change is smaller (< 0.2%), therefore has good cycle life, and 1000 circulation volumes of high rate charge-discharge are protected Holdup still can reach 90% or more.Lithium titanate anode is answered compared with traditional Li-C cathode in high power type lithium ion power battery With having advantage, however the theoretical capacity of lithium titanate is only 175mAh/g, affects it 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 material.But it is decomposed since the presence of Ti-O key will lead to the carbonate solvent in electrolyte, generates flatulence, affect Its practical application.
The preparation method of common lithium titanate-composite titania material is: lithium source and titanium source are added during the reaction, The molar ratio of middle elemental lithium and titanium elements is less than the stoichiometric ratio in lithium titanate, due to the presence of excessive Ti, generates lithium titanate- Composite titania material, lithium titanate and titanium dioxide mutually mix in composition, and the defect of this method is the mixing of lithium titanate Uniformity is poor, and the presence of excess Ti is easy to generate other impurities compound, influences properties of product.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of in-situ preparation lithium titanate-composite titania materials And preparation method thereof, which has nucleocapsid structure, and coated by titanium dioxide is in the outer of lithium titanate Surface, outermost layer coat carbon-coating；It can not only inhibit product flatulence, moreover it is possible to make product that there is good security performance and stable structure Performance.
For this purpose, 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, Middle layer is titanium dioxide, and outermost layer is carbon.
It is preferred that lithium titanate layer with a thickness of micron order, titanium dioxide layer with a thickness of submicron order, carbon layers having thicknesses are nanoscale.
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, comprising the following steps:
1) titanium dioxide is added in sodium hydrate aqueous solution, is kept the temperature in hydrothermal reaction kettle, at 180~210 DEG C anti- 18~48h is answered, material I is obtained；
Wherein the molar ratio of titanium dioxide and sodium hydroxide is 1:(6~24)；
2) the material I is added to 0.4~0.8mol/L [H+] acid solution in, wherein material I described in 1g it is corresponding 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 wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1~2mol/l, hydrothermal reaction kettle is added after mixing, At 150~200 DEG C heat preservation 12~for 24 hours, obtain ion exchange solution II；
5) the ion exchange solution II is washed into supercentrifuge separation, collects solid, obtains material III；
6) the material III is once roasted at 750~800 DEG C, calcining time be 8~for 24 hours, obtain lithium titanate Material；
7) ball milling in sand mill is added in the lithium titanate material, organic carbon source and deionized water, obtains material IV；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 being subjected to after baking under nitrogen or inert gas shielding atmosphere, maturing temperature is 750~ 850 DEG C, calcining time be 6~12h to get arrive the in-situ preparation lithium titanate-composite titania material.
Further, the step 2) acid solution is hydrochloric acid or sulfuric acid.
Further, the step 7) organic carbon source is phenolic resin or polyvinylpyrrolidone.
Further, the step 9) inert gas is helium or argon gas.
The present invention provides a kind of in-situ preparation lithium titanate-composite titania material and preparation method thereof, the lithium titanate- The nucleocapsid structure for being structurally characterized in that two layers of cladding of composite titania material；Wherein outermost layer is carbon, middle layer is titanium dioxide Titanium, innermost layer are lithium titanate.Carbon-coating ensure that composite material has good electric conductivity, and titanium dioxide layer ensure that composite material With higher specific capacity, 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 high temperature solid-state occurs for the carbon source and lithium titanate that cladding is secondly added Reaction；The effect of carbon source mainly has following three points: 1. improving composite material electron conduction, 2. inhibits composite material flatulence, 3. Meeting generating portion lithia steam during carbon coating, enables lithium titanate surface layer that exploded occurs, and generates titanium dioxide/titanium acid lithium Nucleocapsid structure.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of in-situ preparation lithium titanate-composite titania material provided by the invention；
Fig. 2 is the lithium titanate of in-situ preparation made from embodiment 1-composite titania material object phase (XRD) figure.
Specific embodiment
Technical solution of the present invention is described in detail below in conjunction with attached drawing.
Embodiment 1
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, includes the following steps:
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is kept the temperature at 180 DEG C 48h obtains material I；
Wherein the molar ratio of titanium dioxide and sodium hydroxide is 1:6；
2) material I is added to 0.4mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solution=1g/200ml, instead It is 48h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1mol/l, hydrothermal reaction kettle is added after mixing, at 150 DEG C Lower heat preservation for 24 hours, obtains ion exchange solution II；
5) ion exchange solution II is washed to separation in supercentrifuge, solid is collected, obtains material III；
6) material III is once roasted at 750 DEG C, calcining time is for 24 hours, to obtain lithium titanate material；
7) ball milling in sand mill is added in lithium titanate material, phenolic resin and deionized water, 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 subjected to after baking under nitrogen atmosphere, maturing temperature is 750 DEG C, calcining time be 12h to get To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because of after baking shape At titanium dioxide layer.
Embodiment 2
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, includes the following steps:
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is kept the temperature at 210 DEG C 18h obtains material I；
Wherein the molar ratio of titanium dioxide and sodium hydroxide is 1:12；
2) material I is added to 0.8mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solution=1g/100ml, instead It is 12h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after mixing, at 200 DEG C Lower heat preservation 12h, obtains ion exchange solution II；
5) ion exchange solution II is washed to separation in supercentrifuge, solid is collected, obtains material III；
6) material III is once roasted at 800 DEG C, calcining time 8h obtains lithium titanate material；
7) ball milling in sand mill, polyvinylpyrrolidine is added in lithium titanate material, polyvinylpyrrolidone and deionized water 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 subjected to after baking under helium atmosphere, maturing temperature is 800 DEG C, calcining time be 10h to get To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because of after baking shape At titanium dioxide layer.
Embodiment 3
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is kept the temperature at 200 DEG C 36h obtains material I；
Wherein the molar ratio of titanium dioxide and sodium hydroxide is 1:18；
2) material I is added to 0.8mol/L [H+] sulfuric acid solution in, wherein material I/ acid solution=1g/150ml, instead It is 36h between seasonable, obtains ion exchange solution I；
3) ion exchange solution I is put into wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after mixing, at 180 DEG C Lower heat preservation 18h, obtains ion exchange solution II；
5) ion exchange solution II is washed to separation in supercentrifuge, solid is collected, obtains material III；
6) material III is once roasted at 800 DEG C, calcining time 12h obtains lithium titanate material；
7) ball milling in sand mill, polyvinylpyrrolidine is added in lithium titanate material, polyvinylpyrrolidone and deionized water 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 subjected to after baking under argon atmosphere, maturing temperature is 800 DEG C, calcining time be 10h to get To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because of after baking shape At titanium dioxide layer.
Embodiment 4
A kind of preparation method of in-situ preparation lithium titanate-composite titania material, includes the following steps:
1) titanium dioxide is added to the sodium hydroxide solution of 10mol/l, in hydrothermal reaction kettle, is kept the temperature at 200 DEG C 48h obtains material I；
Wherein the molar ratio of titanium dioxide and sodium hydroxide is 1:24；
2) material I is added to 0.8mol/L [H+] hydrochloric acid solution in, wherein material I/ acid solution=1g/200ml, instead It is for 24 hours, to obtain ion exchange solution I between seasonable；
3) ion exchange solution I is put into wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 2mol/l, hydrothermal reaction kettle is added after mixing, at 180 DEG C Lower heat preservation for 24 hours, obtains ion exchange solution II；
5) ion exchange solution II is washed to separation in supercentrifuge, solid is collected, obtains material III；
6) material III is once roasted at 750 DEG C, calcining time is for 24 hours, to obtain lithium titanate material；
7) ball milling in sand mill is added in lithium titanate material, phenolic resin and deionized water, 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 subjected to after baking under nitrogen atmosphere, maturing temperature is 800 DEG C, calcining time be 12h to get To final product.
The product innermost layer is lithium titanate, and outermost layer is carbon, is had between lithium titanate and carbon-coating because of after baking shape At titanium dioxide layer.
Experimental conditions:
Fig. 1 is the structural schematic diagram of in-situ preparation lithium titanate-composite titania material produced by the present invention；It can by figure See, outermost layer 1 is cladding carbon material, and middle layer 2 is the anatase titanium dioxide being formed in situ, and innermost layer 3 is spinelle metatitanic acid Lithium.The structure can guarantee product of the present invention specific capacity with higher compared with pure phase lithium titanate, and can effectively inhibit bulging It is swollen.
Table 1, which is listed, is made button cell for the first time using ion secondary battery cathode material lithium made from 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 ICP053048,5C, 2.0~2.9V, and the charging/discharging apparatus used is blue electricity Charge and discharge instrument.
2 cycle performance of table tests table
As can be seen from the data in the table, lithium titanate anode material cycle performance prepared by the present invention is fine, after 1000 weeks Capacity retention ratio is still 100% or more, and due to carbon-coated effect, and there is no bulging phenomenons.
Fig. 2 is the lithium titanate of in-situ preparation made from example 2-composite titania material object phase (XRD) figure, You Tuke To find out the composite material being prepared based on lithium titanate, with the presence of a small amount of anatase titanium dioxide, since carbon is amorphous State and content is lower, therefore exist without carbon peak.

Claims (5)

1. a kind of preparation method of in-situ preparation lithium titanate-composite titania material, it is characterised in that the following steps are included:
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 molar ratio of titanium dioxide and sodium hydroxide is 1:6~24；
2) the material I is added to 0.4~0.8mol/L [H+] acid solution in, wherein material I described in 1g is corresponding is added 100 Acid solution described in~200ml, reaction time are 12~48h, obtain ion exchange solution I；
3) the ion exchange solution I is put into wash in supercentrifuge and is separated, collected solid, obtain material II；
4) material II is added to the lithium hydroxide solution of 1~2mol/l, hydrothermal reaction kettle is added after mixing, 150~ At 200 DEG C heat preservation 12~for 24 hours, obtain ion exchange solution II；
5) the ion exchange solution II is washed into supercentrifuge separation, collects solid, obtains material III；
6) the material III is once roasted at 750~800 DEG C, calcining time be 8~for 24 hours, obtain lithium titanate material Material；
7) ball milling in sand mill is added in the lithium titanate material, organic carbon source and deionized water, obtains material IV；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 being subjected to after baking under nitrogen or inert gas shielding atmosphere, maturing temperature is 750~850 DEG C, Calcining time be 6~12h to get arrive the in-situ preparation lithium titanate-composite titania material；
In-situ preparation lithium titanate-the composite titania material has nucleocapsid structure, is divided into three layers from inside to outside, innermost layer It is titanium dioxide for lithium titanate, middle layer, outermost layer is carbon.
2. the preparation method of in-situ preparation lithium titanate-composite titania material as described in claim 1, it is characterised in that: step Rapid 2) the described acid solution is hydrochloric acid or sulfuric acid.
3. the preparation method of in-situ preparation lithium titanate-composite titania material as described in claim 1, it is characterised in that: step Rapid 7) the described organic carbon source is phenolic resin or polyvinylpyrrolidone.
4. the preparation method of in-situ preparation lithium titanate-composite titania material as described in claim 1, it is characterised in that: step Rapid 9) the described inert gas is helium or argon gas.
5. the preparation method of in-situ preparation lithium titanate-composite titania material as described in claim 1, it is characterised in that: system In-situ preparation lithium titanate-composite titania material lithium titanate the layer obtained is with a thickness of micron order, titanium dioxide layer with a thickness of Asia Micron order, carbon layers having thicknesses are nanoscale.
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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
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WO2014194996A1 (en) * 2013-06-05 2014-12-11 Clariant Produkte (Deutschland) Gmbh Process for the preparation of lithium titanium spinel and its use
CN105206815A (en) * 2015-09-28 2015-12-30 清华大学 Carbon-coated Li4Ti5O12-TiO2/Sn nanocomposite and preparation and application thereof

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WO2014194996A1 (en) * 2013-06-05 2014-12-11 Clariant Produkte (Deutschland) Gmbh Process for the preparation of lithium titanium spinel and its use
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