CN108365206A - A method of preparing NiO cladding lithium titanate composite anode materials - Google Patents

A method of preparing NiO cladding lithium titanate composite anode materials Download PDF

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Publication number
CN108365206A
CN108365206A CN201810224326.0A CN201810224326A CN108365206A CN 108365206 A CN108365206 A CN 108365206A CN 201810224326 A CN201810224326 A CN 201810224326A CN 108365206 A CN108365206 A CN 108365206A
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lithium titanate
nio
room temperature
temperature
composite anode
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黄技军
赵东辉
周鹏伟
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Fujian Xfh Battery Material Co Ltd
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Fujian Xfh Battery Material 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/485—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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention discloses a kind of method preparing NiO cladding lithium titanate composite anode materials, and using high temperature process heat, step is：Weigh potassium carbonate and titanium dioxide, alleged material be put into room temperature Muffle furnace, heating rate is 5 °/min, to 800 DEG C of predetermined temperature after constant temperature 18 hours；It takes out after the heat preservation predetermined time, cools down at room temperature；The nano NiO that mass percent is 0.5 3% is added again.The present invention is synthetically prepared lithium titanate using high temperature solid-state method, high temperature solid-state method has the reaction time short, it is simple for process, easily realize industrialization large-scale production and the quick major advantage of combustion synthesis reaction, it can obtain the product of crystal perfection in a relatively short period of time again, it is suitable for the mass production of lithium titanate and the present invention coats it using nickel oxide, improves the charge specific capacity of lithium titanate.

Description

A method of preparing NiO cladding lithium titanate composite anode materials
Technical field
The present invention relates to negative material field technology, refer in particular to a kind of preparing NiO cladding lithium titanate composite anode materials Method.
Background technology
With the fast development of emerging economies, global energy consumption sharp increase.Lithium ion battery is with its high voltage, height Energy density, the advantages that having extended cycle life, have a safety feature, is of low cost, are in portable electrics such as computer, camera and mobile phones It has been obtained for being widely applied in sub- equipment.In recent years, countries in the world all apply to mix actively developing lithium ion battery Power electric automobile（HEV）, pure electric automobile（PEV）Deng research, but lithium ion battery is as the main of vehicle mounted dynamic battery Bottleneck is the performance of lithium ion battery negative material.
The lithium titanate of spinel-type has very high structural stability and longer cycle life, has application prospect One of lithium ion battery negative material.Lithium titanate has higher intercalation potential in charge and discharge process, can avoid Li dendrite There is the formation with SEI films, and its volume in charge and discharge process is almost unchanged, therefore is referred to as " zero strain material ".However, The electronic conductivity of lithium titanate is relatively low and lithium titanate specific capacity is relatively low with respect to mainstream negative material graphite.
Chinese invention patent application publication No. CN 105226263A disclose a kind of preparation side of lithium titanate lithium ion battery Method and application, method are：
1), the preparation of solvent：Polyethylene glycol, magnesium acetate are pressed 1:l~1:It is fully dissolved in pure water after 5 mass ratio mixing；
2), the preparation of solute：By Ag, Co, Mg, Ti, Si, one or more of compound of Zr is mixed with nano-titanium dioxide It closes, the mass percent that nanometer titanium dioxide is admired after mixing is 10% one 30%；
3) manufactured solute in step 2, is dissolved in the solvent in step 1) and obtains suspension;
4) suspension in step 3, is subjected to ultraviolet light；
5), by step 4 treated suspension together with metatitanic acid, lithium source, dispersant ball milling, be carried out at the same time ultraviolet light；
6）, will be through step 5）What is dried after levigate and mixing obtains lithium titanate material.
There are processing step complexity for the above method.
Invention content
In view of this, preparing NiO claddings in view of the deficiencies of the prior art, the present invention aims to provide a kind of The method of lithium titanate composite anode material can improve production efficiency, reduce manufacturing cost, quickly and effectively prepare product and carry The cycle performance and capacity retention ratio of high battery.
To achieve the above object, the present invention is using following technical solution：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh carbon Alleged material is put into room temperature Muffle furnace by sour potassium and titanium dioxide, and heating rate is 5 °/min, arrives perseverance after 800 DEG C of predetermined temperature It is 1-8 hours warm；It takes out after the heat preservation predetermined time, cools down at room temperature；The nano NiO that mass percent is 0.5-3% is added again.
As a preferred embodiment, the nano NiO is prepared using fused salt combustion method, nickel acetate is weighed, by alleged acetic acid Nickel is put into room temperature Muffle furnace, and heating rate is 5 °/min, to 500-800 DEG C of predetermined temperature after constant temperature 2-10 hours；Heat preservation is predetermined It takes out after time, cools down at room temperature.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal Known to：
The present invention is synthetically prepared lithium titanate using high temperature solid-state method, and high temperature solid-state method has the reaction time short, simple for process, Yi Shi Existing industrialization large-scale production and the quick major advantage of combustion synthesis reaction, but it is complete to obtain crystal in a relatively short period of time Whole product, is suitable for the mass production of lithium titanate and this patent coats it using nickel oxide, improves metatitanic acid The charge specific capacity of lithium.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of the obtained NiO cladding lithium titanates of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of the obtained NiO cladding lithium titanates of the present invention；
Fig. 3 is the cycle performance figure of the obtained NiO cladding lithium titanates of the present invention.
Specific implementation mode
Present invention is disclosed a kind of methods for preparing NiO and coating lithium titanate composite anode material, using high temperature process heat, Its step is：Potassium carbonate and titanium dioxide are weighed, alleged material is put into room temperature Muffle furnace, heating rate is 5 °/min, in advance Constant temperature 1-8 hours after 800 DEG C of constant temperature degree；It takes out after the heat preservation predetermined time, cools down at room temperature；Adding mass percent again is The nano NiO of 0.5-3%.
The nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature Muffle furnace, Heating rate was 5 °/min, to constant temperature after 500-800 DEG C of predetermined temperature 2-10 hours；It is taken out after the heat preservation predetermined time, in room temperature Lower cooling.
With multiple embodiments, invention is further described in detail below：
Embodiment 1：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 8g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace with 5 DEG C/min is preheating to 800 DEG C, in 800 DEG C of constant temperature 4 hours, Heat preservation directly took out crucible after reacting 4 hours from Muffle furnace It is positioned in air and is cooled to room temperature, obtain nano lithium titanate, then add the nano-nickel oxide that mass percent is 2.8%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 600 DEG C of predetermined temperature 6 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
Fig. 1 is the X ray diffracting spectrum of the NiO cladding lithium titanates obtained in the present embodiment, as shown in Figure 1, lithium titanate production Object presents JCPDS, and the structure of No. 26-1198 shows that made sample principal crystalline phase is lithium titanate, zinc oxide do not occur in figure Diffraction maximum, illustrate that small amounts nickel, which is added, does not change the crystal form of lithium titanate, side light nickel oxide is coated on lithium titanate.
Fig. 2 is the scanning electron microscope (SEM) photograph of the NiO cladding lithium titanates obtained in the present embodiment, and made sample is microcosmic as shown in Figure 2 Pattern is nano particle, and NiO cladding lithium titanate nano composite anode materials are prepared under this temperature and time.
Fig. 3 is the cycle performance figure of the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, can be with from figure Find out that the initial charge specific capacity of NiO cladding lithium titanates is 172.3mAh/g, hence it is evident that be higher than the initial charge of uncoated lithium titanate Specific capacity 159.7mAh/g after recycling 40 times, coats its charge specific capacity of the lithium titanate of NiO as 171.5mAh/g, and uncoated Its charge specific capacity is 159mAh/g after the lithium titanate of NiO recycles 40 times, from data, it is apparent that NiO coats lithium titanate Significantly improve its cycle performance.
Embodiment 2：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 7g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace with 5 DEG C/min is preheating to 800 DEG C, in 800 DEG C of constant temperature 1 hour, Heat preservation directly took out crucible after reacting 1 hour from Muffle furnace It is positioned in air and is cooled to room temperature, obtain nano lithium titanate, then add the nano-nickel oxide that mass percent is 0.5%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 500 DEG C of predetermined temperature 2 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
After tested, the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, initial charge specific capacity are 170.3mAh/g, after recycling 40 times, charge specific capacity 169.5mAh/g.
Embodiment 3：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 6g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace with 5 DEG C/min is preheating to 800 DEG C, in 800 DEG C of constant temperature 8 hours, Heat preservation directly took out crucible after reacting 8 hours from Muffle furnace It is positioned in air and is cooled to room temperature, obtain nano lithium titanate, then add the nano-nickel oxide that mass percent is 1.2%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 700 DEG C of predetermined temperature 4 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
After tested, the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, initial charge specific capacity are 168.8mAh/g, after recycling 40 times, charge specific capacity 168.5mAh/g.
Embodiment 4：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 6.5g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace 800 DEG C are preheating to 5 DEG C/min, in 800 DEG C of constant temperature 5 hours, Heat preservation directly took out earthenware after reacting 5 hours from Muffle furnace Pot, which is positioned in air, to be cooled to room temperature, and nano lithium titanate is obtained, then adds the nano-nickel oxide that mass percent is 3%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 800 DEG C of predetermined temperature 8 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
After tested, the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, initial charge specific capacity are 167.9mAh/g, after recycling 40 times, charge specific capacity 166.8mAh/g.
Embodiment 5：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 7.4g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace 800 DEG C are preheating to 5 DEG C/min, in 800 DEG C of constant temperature 6 hours, Heat preservation directly took out earthenware after reacting 6 hours from Muffle furnace Pot, which is positioned in air, to be cooled to room temperature, and nano lithium titanate is obtained, then adds the nano-nickel oxide that mass percent is 2.2%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 550 DEG C of predetermined temperature 10 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
After tested, the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, initial charge specific capacity are 167.7mAh/g, after recycling 40 times, charge specific capacity 166.8mAh/g.
Embodiment 6：
A method of NiO cladding lithium titanate composite anode materials being prepared, using high temperature process heat, step is：Weigh by The potassium carbonate and titanium dioxide 6.5g of certain stoichiometric ratio are positioned in 300 mL crucibles, then, are put into room temperature Muffle furnace 800 DEG C are preheating to 5 DEG C/min, in 800 DEG C of constant temperature 7 hours, Heat preservation directly took out earthenware after reacting 7 hours from Muffle furnace Pot, which is positioned in air, to be cooled to room temperature, and nano lithium titanate is obtained, then adds the nano-nickel oxide that mass percent is 2.8%.
Wherein, the nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature horse Not stove, heating rate were 5 °/min, to constant temperature after 650 DEG C of predetermined temperature 6 hours；It is taken out after the heat preservation predetermined time, at room temperature It is cooling.
After tested, the NiO cladding lithium titanate composite anode materials obtained in the present embodiment, initial charge specific capacity are 167.1mAh/g, after recycling 40 times, charge specific capacity 166.5mAh/g.
The design focal point of the present invention is：The present invention is synthetically prepared lithium titanate, high temperature solid-state method tool using high temperature solid-state method Have that the reaction time is short, it is simple for process, easily realize industrialization large-scale production and the quick major advantage of combustion synthesis reaction, and energy The product that can obtain crystal perfection in a relatively short period of time, is suitable for the mass production of lithium titanate and this patent is using oxidation Nickel coats it, improves the charge specific capacity of lithium titanate.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention, Therefore it is every according to the technical essence of the invention to any subtle modifications, equivalent variations and modifications made by above example, still Belong in the range of technical solution of the present invention.

Claims (2)

1. a kind of method preparing NiO cladding lithium titanate composite anode materials, it is characterised in that：Using high temperature process heat, Step is：Potassium carbonate and titanium dioxide are weighed, alleged material is put into room temperature Muffle furnace, heating rate is 5 °/min, is arrived predetermined Constant temperature 1-8 hours after 800 DEG C of temperature；It takes out after the heat preservation predetermined time, cools down at room temperature；It is 0.5- to add mass percent again 3% nano NiO.
2. a kind of method preparing NiO cladding lithium titanate composite anode materials according to claim 1, it is characterised in that： The nano NiO is prepared using fused salt combustion method, weighs nickel acetate, alleged nickel acetate is put into room temperature Muffle furnace, heating rate For 5 °/min, to 500-800 DEG C of predetermined temperature after constant temperature 2-10 hours；It takes out after the heat preservation predetermined time, cools down at room temperature.
CN201810224326.0A 2018-03-19 2018-03-19 A method of preparing NiO cladding lithium titanate composite anode materials Pending CN108365206A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109524660A (en) * 2018-11-22 2019-03-26 成都先进金属材料产业技术研究院有限公司 It adds purification ultrafine titanium powder preparation and contains Ti3+The method of lithium titanate

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN103337616A (en) * 2013-06-28 2013-10-02 上海电力学院 Metal oxide coated lithium titanate negative pole material and preparation method thereof
CN104425808A (en) * 2013-08-26 2015-03-18 华为技术有限公司 Lithium ion battery composite anode material and preparation method thereof and lithium ion battery
CN107792890A (en) * 2017-09-15 2018-03-13 福建翔丰华新能源材料有限公司 The method for preparing nano NiO lithium ion battery negative material

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Publication number Priority date Publication date Assignee Title
CN103337616A (en) * 2013-06-28 2013-10-02 上海电力学院 Metal oxide coated lithium titanate negative pole material and preparation method thereof
CN104425808A (en) * 2013-08-26 2015-03-18 华为技术有限公司 Lithium ion battery composite anode material and preparation method thereof and lithium ion battery
CN107792890A (en) * 2017-09-15 2018-03-13 福建翔丰华新能源材料有限公司 The method for preparing nano NiO lithium ion battery negative material

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杨双磊: "锂离子电池电极材料的制备及其电化学性能研究", 《中国优秀硕士学位论文全文数据库•工程科技Ⅱ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109524660A (en) * 2018-11-22 2019-03-26 成都先进金属材料产业技术研究院有限公司 It adds purification ultrafine titanium powder preparation and contains Ti3+The method of lithium titanate

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