CN105226263A - The preparation method of lithium titanate - Google Patents

The preparation method of lithium titanate Download PDF

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Publication number
CN105226263A
CN105226263A CN201510678429.0A CN201510678429A CN105226263A CN 105226263 A CN105226263 A CN 105226263A CN 201510678429 A CN201510678429 A CN 201510678429A CN 105226263 A CN105226263 A CN 105226263A
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CN
China
Prior art keywords
preparation
lithium titanate
suspension
lithium
solvent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510678429.0A
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Chinese (zh)
Inventor
李延俊
岳波
向中林
王俊安
周俊杰
颜宇强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SICHUAN KENENG LITHIUM BATTERY Co Ltd
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SICHUAN KENENG LITHIUM BATTERY Co Ltd
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Priority to CN201510678429.0A priority Critical patent/CN105226263A/en
Publication of CN105226263A publication Critical patent/CN105226263A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • H01M4/1391Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028Positive electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00Batteries for particular applications
    • H01M2220/20Batteries in motive systems, e.g. vehicle, ship, plane
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00Batteries for particular applications
    • H01M2220/30Batteries in portable systems, e.g. mobile phone, laptop
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

1), the preparation of solvent the present invention relates to the preparation method of lithium titanate, comprise the following steps:: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1 ~ 1:5; 2), the preparation of solute: one or more in the compound of Ag, Co, Mg, Ti, Si, Zr mixed with nano titanium oxide, after mixing, the mass percent of nano titanium oxide is 10% ~ 30%; 3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension; 4), the suspension in step 3) is carried out UV-irradiation; 5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously; 6), by through step 5) levigate and mix post-drying obtain lithium titanate material.Lithium titanate material prepared by the present invention is applied to lithium battery discharge performance that positive electrode makes, stability is good.

Description

The preparation method of lithium titanate
Technical field
The present invention relates to lithium battery material field, particularly, relate to a kind of preparation method of lithium titanate.
Background technology
Along with the fast development of traffic, communication and the industrialization of information, the products such as electric automobile, notebook computer and mobile communications tool propose higher and very urgent requirement to Development of Novel chemical power source.Development of new secondary green battery has become and must need.Lithium ion battery is relative to traditional secondary battery, due to its have that energy density is high, power density is high, operating voltage is high, self-discharge rate is low, memory-less effect, have extended cycle life, the unique advantage such as pollution-free, become rapidly a kind of most important and state-of-the-art secondary cell.Having become the ideal source of the electronic installation miniaturization ands such as video camera, mobile phone, notebook computer and portable surveying instrument, is also the first-selected power supply of following light high-energy electrokinetic cell used for electric vehicle.
At present, in commercial Li-ion battery, great majority adopt carbon electrode as negative material.But because the current potential in the current potential of carbon electrode after slotting lithium and metal is very close, and most electrolyte is unstable under this current potential, and electrolyte easily decomposes at electrode surface.So when over-charging of battery, carbon electrodes easily separates out very active lithium metal, form the dendrite of lithium, the danger that barrier film causes short circuit may be pierced through, and the thermal runaway that high temperature is, affect the security performance of battery.Researcher is also to the negative material of other many lithium-ions battery, as lithium alloy, oxide, sulfide and high molecular polymer etc. are explored, at present, these materials are all undesirable, some can not solve the hidden danger in safety, and some is then that cycle performance is too poor etc.Therefore, finding the new negative material substituting carbon electrode is, one of Main way of research at present.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method with high-rate discharge ability, lithium titanate that stability is good.
The present invention's adopted technical scheme that solves the problem is: the preparation method of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1 ~ 1:5;
2), the preparation of solute: one or more in the compound of Ag, Co, Mg, Ti, Si, Zr mixed with nano titanium oxide, after mixing, the mass percent of nano titanium oxide is 10% ~ 30%;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously;
6), by through step 5) levigate and mix post-drying obtain lithium titanate material.
Further, polyethylene glycol, magnesium acetate be 1:2 ~ 1:3 in mass percent.
Further, the compound of Ag, Co, Mg, Ti, Si, Zr is nitrate, fluoride, acetate, oxide or lipoid substance.
Further, the granularity of titanium dioxide is 50 ~ 100nm.
Further, dispersant is polyvinyl alcohol.
Further, the temperature of oven dry is 600 DEG C ~ 800 DEG C.
To sum up, the invention has the beneficial effects as follows:
1, of the present invention simple to operate, and environmentally friendly, reduce production cost, be easy to suitability for industrialized production.
2, the lithium titanate material that prepared by the present invention is applied to lithium battery discharge performance that positive electrode makes, stability is good.
Embodiment
Below in conjunction with embodiment, to the detailed description further of invention do, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation method of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1;
2), the preparation of solute: the one in silver nitrate mixed with nano titanium oxide, after mixing, the mass percent of nano titanium oxide is 10%; The granularity of titanium dioxide is 50nm;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously; Described dispersant is polyvinyl alcohol;
6), by through step 5) levigate and mixing after at 600 DEG C dry obtain lithium titanate material.
Embodiment 2:
The preparation method of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:2;
2), the preparation of solute: the one in silver nitrate mixed with nano titanium oxide, after mixing, the mass percent of nano titanium oxide is 20%; The granularity of titanium dioxide is 80nm;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously; Described dispersant is polyvinyl alcohol;
6), by through step 5) levigate and mixing after at 700 DEG C dry obtain lithium titanate material.
Embodiment 3:
The preparation method of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:3;
2), the preparation of solute: the one in silver nitrate is mixed with nano titanium oxide, the percent mass 30% of nano titanium oxide after mixing; The granularity of titanium dioxide is 100nm;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously; Described dispersant is polyvinyl alcohol;
6), by through step 5) levigate and mixing after at 800 DEG C dry obtain lithium titanate material.
Embodiment 4:
The preparation method of lithium titanate, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:5;
2), the preparation of solute: the one in silver nitrate is mixed with nano titanium oxide, the percent mass 30% of nano titanium oxide after mixing; The granularity of titanium dioxide is 100nm;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously; Described dispersant is polyvinyl alcohol;
6), by through step 5) levigate and mixing after at 800 DEG C dry obtain lithium titanate material.
As mentioned above, the present invention can be realized preferably.

Claims (6)

1. the preparation method of lithium titanate, is characterized in that, comprises the following steps:
1), the preparation of solvent: polyethylene glycol, magnesium acetate are all dissolved in pure water by after the mass ratio mixing of 1:1 ~ 1:5;
2), the preparation of solute: one or more in the compound of Ag, Co, Mg, Ti, Si, Zr mixed with nano titanium oxide, after mixing, the mass percent of nano titanium oxide is 10% ~ 30%;
3), by step 2) in the solvent of solute dissolves in step 1) made obtain suspension;
4), the suspension in step 3) is carried out UV-irradiation;
5), by the suspension after step 4) process together with metatitanic acid, lithium source, dispersant ball milling, carry out UV-irradiation simultaneously;
6), by through step 5) levigate and mix post-drying obtain lithium titanate material.
2. the preparation method of lithium titanate according to claim 1, is characterized in that, described polyethylene glycol, magnesium acetate be 1:2 ~ 1:3 in mass percent.
3. the preparation method of lithium titanate according to claim 1, is characterized in that, the compound of described Ag, Co, Mg, Ti, Si, Zr is nitrate, fluoride, acetate, oxide or lipoid substance.
4. the preparation method of lithium titanate according to claim 1, is characterized in that, the granularity of described titanium dioxide is 50 ~ 100nm.
5. the preparation method of lithium titanate according to claim 1, is characterized in that, described dispersant is polyvinyl alcohol.
6., according to the preparation method of the arbitrary described lithium titanate of claim 1 to 5, it is characterized in that, the temperature of described oven dry is 600 DEG C ~ 800 DEG C.
CN201510678429.0A 2015-10-20 2015-10-20 The preparation method of lithium titanate Pending CN105226263A (en)

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Publications (1)

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CN105226263A true CN105226263A (en) 2016-01-06

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040018431A1 (en) * 2001-07-27 2004-01-29 A123 Systems, Inc. Battery structures and related methods
CN103441257A (en) * 2013-08-12 2013-12-11 四川大学 Preparation method for lithium titanate material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040018431A1 (en) * 2001-07-27 2004-01-29 A123 Systems, Inc. Battery structures and related methods
CN103441257A (en) * 2013-08-12 2013-12-11 四川大学 Preparation method for lithium titanate material

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Application publication date: 20160106