CN106159250A - A kind of metatitanic acid is the lithium titanate electrode material in titanium source and preparation method thereof - Google Patents
A kind of metatitanic acid is the lithium titanate electrode material in titanium source and preparation method thereof Download PDFInfo
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- CN106159250A CN106159250A CN201610668773.6A CN201610668773A CN106159250A CN 106159250 A CN106159250 A CN 106159250A CN 201610668773 A CN201610668773 A CN 201610668773A CN 106159250 A CN106159250 A CN 106159250A
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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
- H01M4/48—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
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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
- 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
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Abstract
The present invention relates to technical field of lithium batteries, be specifically related to lithium titanate electrode material that a kind of metatitanic acid is titanium source and preparation method thereof, raw material includes metatitanic acid TiO (OH)2, lithium salts LixM and metal nitrate salt additives RyNO3, wherein, Li:Ti=0.8 0.85:1, R:Ti=0.015 0.025:1, described M are carbanion or hydroxide ion, and R is metal ion, and x is 12, and y is 0.25 1；By by metatitanic acid, lithium salts and metal nitrate salt additives mixing and stirring, it is dried, calcining, cooling, obtains lithium titanate electrode material.The present invention prepares lithium titanate electrode material with the intermediate metatitanic acid of titanium dioxide for titanium source, the lithium titanate electrode material prepared is made to possess the charge-discharge performance of excellence, meet the requirement of lithium ion battery negative material, and preparation method is simple, preparation cost is low, the lithium titanate electrode material excellent performance prepared, significant to the application development promoting lithium battery.
Description
Technical field
The present invention relates to technical field of lithium batteries, be specifically related to lithium titanate electrode material that a kind of metatitanic acid is titanium source and
Preparation method.
Background technology
Lithium ion battery has had been widely used for mobile phone, notebook computer, digital camera etc. since commercialization in 1991
Various portable electronics.In recent years, along with hybrid vehicle and the fast development of pure electric automobile, people are to as power current
The capacity of the lithium ion battery in source, cycle life and safety propose requirements at the higher level.
At present, the negative active core-shell material of commercial Li-ion battery is mainly various graphite carbon material, and graphite cathode
Under the conditions of high current charge-discharge, easily separate out Li dendrite, there is potential safety hazard.Compared with graphite negative electrodes material, spinelle is tied
The lithium titanate Li of structure4Ti5O12Have as lithium ion battery negative material that cycle life is longer and the higher advantage of safety, because of
And cause people and pay close attention to greatly and pay attention to.
The raw material of preparing of lithium titanate includes lithium source and titanium source, and titanium dioxide is former frequently as preparing lithium titanate with spinel structure
Titanium source in material, as China Patent No. CN201510170549.X discloses the preparation method of a kind of lithium titanate material, lithium titanate
Cathode pole piece and lithium ion battery, titanium source wherein used is nano titanium oxide, China Patent No. CN 201410673307.8
Disclosing a kind of preparation method preparing carbon cladding lithium titanate anode material, titanium source used is titanium dioxide, prepares lithium titanate
Required titanium dioxide is Detitanium-ore-type, and the most existing titanium dioxide is used for the necks such as paint, coating, fine ceramics
Territory, major part is pigmentary rutile titanium dioxide, the technical maturity of rutile TiO_2, and lot stability is good, and right
In the anatase titanium dioxide that lithium electricity is special, consumption is less, and technique is immature, and therefore, in raw material, anatase type tio2 criticizes
Secondary stability is bad, causes the lithium titanate lot stability produced poor, also affects the performance of lithium titanate chemical property.
Summary of the invention
It is an object of the invention to solve above technical problem, it is provided that a kind of metatitanic acid is the lithium titanate electrode material in titanium source
And preparation method thereof, prepare lithium titanate electrode material with the intermediate metatitanic acid of titanium dioxide for titanium source, make the lithium titanate prepared
Electrode material possesses the charge-discharge performance of excellence, meets the requirement of lithium ion battery negative material.
For solve the problems referred to above, the present invention by the following technical solutions:
A kind of metatitanic acid is the lithium titanate electrode material in titanium source, and raw material includes metatitanic acid TiO (OH)2, lithium salts LixM and metal
Nitrate additive RyNO3, wherein, Li:Ti=0.8-0.85:1, R:Ti=0.015-0.025:1, described M is carbanion
Or hydroxide ion, R is metal ion, x be 1-2, y be 0.25-1.
Further, the solid content of described metatitanic acid is 30%-60%.
Further, at least one during described lithium salts is lithium carbonate and Lithium hydrate.
Further, at least one during described metal nitrate salt additives is the metal nitrate of Mg, Zr, Na, Zn.
Above-mentioned metatitanic acid is the preparation method of the lithium titanate electrode material in titanium source, comprises the following steps: by metatitanic acid, lithium salts
With metal nitrate salt additives mixing and stirring, it is dried, calcining, cooling, obtains lithium titanate electrode material.
Further, the described mix and blend time is 1-3h.
Further, described being dried is carried out by least one in spray drying, vacuum drying, forced air drying.
Further, twice firing at pre-burning and 700-900 DEG C at described calcining is included in 400-600 DEG C.
Further, the time of described pre-burning is 1-6h, and the time of twice firing is 1-6h.
The raw material of lithium titanate electrode material of the present invention includes metatitanic acid TiO (OH)2, lithium salts LixM and metal nitrate add
Agent RyNO3, wherein, the mol ratio of Li and Ti be the mol ratio of 0.8-0.85:1, R and Ti be 0.015-0.025:1, raw material is mixed
Conjunction stirs, and is dried, calcining, and cooling obtains lithium titanate electrode material.
A kind of metatitanic acid of the present invention is the lithium titanate electrode material in titanium source and preparation method thereof, compared with prior art, and its
Prominent feature and excellent effect are:
1. the present invention prepares lithium titanate electrode material with the intermediate metatitanic acid of titanium dioxide for titanium source, makes the metatitanic acid prepared
Lithium electrode material possesses the charge-discharge performance of excellence, meets the requirement of lithium ion battery negative material.
2. the lithium titanate electrode material of the present invention is the lithium titanate anode material of spinel structure, has high power capacity, high power concurrently
Rate and excellent charge-discharge performance.
3. the preparation method of the present invention is simple, and preparation cost is low, and the lithium titanate electrode material excellent performance prepared, to promotion
The application development of lithium battery is significant.
Accompanying drawing explanation
Fig. 1 is the charging and discharging curve of the lithium titanate electrode material that embodiment 5 obtains；
Fig. 2 is the cyclic curve of the lithium titanate electrode material that embodiment 5 obtains；
Fig. 3 is the lithium titanate electrode material that obtains of embodiment 3 and the discharge-rate curve of pure phase lithium titanate.
Detailed description of the invention
Below by way of detailed description of the invention and accompanying drawing, the present invention is described in further detail, but should this be interpreted as
The scope of the present invention is only limitted to Examples below.In the case of without departing from said method thought of the present invention, general according to this area
Various replacements that logical technological know-how and customary means are made or change, should be included in the scope of the present invention.
Embodiment 1
A kind of metatitanic acid is the lithium titanate electrode material in titanium source: raw material includes metatitanic acid TiO (OH)2, lithium carbonate Li2CO3With
Magnesium nitrate Mg (NO3)2, wherein, Li:Ti=0.8-0.85:1, Mg:Ti=0.015:1, by raw material mix and blend 1h, spray dried
Dry, pre-burning 6h at 400 DEG C, then twice firing 6h at 700 DEG C, cooling, obtain lithium titanate electrode material；Described metatitanic acid
Solid content be 30%.
Embodiment 2
A kind of metatitanic acid is the lithium titanate electrode material in titanium source: raw material includes metatitanic acid TiO (OH)2, lithium carbonate Li2CO3、
Lithium hydrate LiOH, sodium nitrate NaNO3With zinc nitrate Zn (NO3)2, wherein, Li:Ti=0.85:1, (Na+Zn): Ti=0.025:
1, by raw material mix and blend 3h, vacuum drying, pre-burning 1h at 600 DEG C, then twice firing 1h at 900 DEG C, cooling, obtain
Lithium titanate electrode material；The solid content of described metatitanic acid is 60%.
Embodiment 3
A kind of metatitanic acid is the lithium titanate electrode material in titanium source: raw material includes metatitanic acid TiO (OH)2, lithium carbonate Li2CO3With
Zirconium nitrate Zr (NO3)4, wherein, Li:Ti=0.82:1, Zr:Ti=0.02:1, by raw material mix and blend 3h, forced air drying,
Pre-burning 2h at 500 DEG C, then twice firing 3h at 800 DEG C, cooling, obtain lithium titanate electrode material；Consolidating of described metatitanic acid
Content is 40%.
Embodiment 4
A kind of metatitanic acid is the lithium titanate electrode material in titanium source: raw material includes metatitanic acid TiO (OH)2, lithium carbonate Li2CO3、
Magnesium nitrate Mg (NO3)2With zirconium nitrate Zr (NO3)4, wherein, Li:Ti=0.83:1, (Mg+Zr): Ti=0.022:1, mix raw material
Closing stirring 2h, carry out successively being spray-dried, being vacuum dried, pre-burning 3h at 550 DEG C, then twice firing 5h at 700 DEG C, cold
But, lithium titanate electrode material is obtained；The solid content of described metatitanic acid is 48%.
Embodiment 5
A kind of metatitanic acid is the lithium titanate electrode material in titanium source: raw material includes metatitanic acid TiO (OH)2, lithium carbonate Li2CO3With
Zirconium nitrate Zr (NO3)4, wherein, Li:Ti=0.81:1, Zr:Ti=0.018:1, by raw material mix and blend 2.5h, forced air drying,
Pre-burning 2h at 600 DEG C, then twice firing 3h at 800 DEG C, cooling, obtain lithium titanate electrode material；Described metatitanic acid
Solid content is 55%.
Lithium titanate electrode material embodiment 1-5 obtained does specific discharge capacity detection, testing result such as table 1:
The specific discharge capacity detection table of the lithium titanate electrode material of table 1 embodiment 1-5
The lithium titanate electrode material that embodiment 5 obtains is done charge-discharge test, and result such as Fig. 1 and Fig. 2, Fig. 1 are lithium titanate
The charging and discharging curve of electrode material, Fig. 2 is the cyclic curve of lithium titanate electrode material；The lithium titanate electrode that embodiment 3 is obtained
Material and pure phase lithium titanate do discharge-rate test, and result such as Fig. 3, Fig. 3 are putting of lithium titanate electrode material and pure phase lithium titanate
Electricity curve of double curvature.
Claims (9)
1. a metatitanic acid is the lithium titanate electrode material in titanium source, it is characterised in that raw material includes metatitanic acid TiO (OH)2, lithium salts
LixM and metal nitrate salt additives RyNO3, wherein, Li:Ti=0.8-0.85:1, R:Ti=0.015-0.025:1, described M is
Carbanion or hydroxide ion, R is metal ion, x be 1-2, y be 0.25-1.
A kind of metatitanic acid the most according to claim 1 is the lithium titanate electrode material in titanium source, it is characterised in that described inclined titanium
The solid content of acid is 30%-60%.
A kind of metatitanic acid the most according to claim 1 is the lithium titanate electrode material in titanium source, it is characterised in that described lithium salts
For at least one in lithium carbonate and Lithium hydrate.
A kind of metatitanic acid the most according to claim 1 is the lithium titanate electrode material in titanium source, it is characterised in that described metal
Nitrate additive is at least one in the metal nitrate of Mg, Zr, Na, Zn.
5. a metatitanic acid as claimed in claim 1 is the preparation method of lithium titanate electrode material in titanium source, it is characterised in that bag
Include following steps: by metatitanic acid, lithium salts and metal nitrate salt additives mixing and stirring, be dried, calcining, cooling, obtain titanium
Acid lithium electrode material.
A kind of metatitanic acid the most according to claim 5 is the preparation method of the lithium titanate electrode material in titanium source, and its feature exists
In, the time of described mix and blend is 1-3h.
A kind of metatitanic acid the most according to claim 5 is the preparation method of the lithium titanate electrode material in titanium source, and its feature exists
In, described being dried is carried out by least one in spray drying, vacuum drying, forced air drying.
A kind of metatitanic acid the most according to claim 5 is the preparation method of the lithium titanate electrode material in titanium source, and its feature exists
Twice firing at pre-burning and 700-900 DEG C at, described calcining is included in 400-600 DEG C.
A kind of metatitanic acid the most according to claim 8 is the preparation method of the lithium titanate electrode material in titanium source, and its feature exists
In, the time of described pre-burning is 1-6h, and the time of twice firing is 1-6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092413A (en) * | 2019-05-09 | 2019-08-06 | 云南中烟工业有限责任公司 | A kind of method that spray drying-solid phase method prepares lithium titanate |
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| CN101630732A (en) * | 2009-07-27 | 2010-01-20 | 深圳市德方纳米科技有限公司 | Nanoscale lithium titanate compound and preparation method thereof |
| WO2012020998A2 (en) * | 2010-08-11 | 2012-02-16 | 주식회사 루트제이제이 | Method for preparing lithium titanium oxide, lithium titanium oxide prepared by same, and lithium secondary battery comprising the lithium titanium oxide |
| CN105406051A (en) * | 2014-09-16 | 2016-03-16 | 河南科隆新能源有限公司 | Composite lithium titanate preparation method |
| CN105470490A (en) * | 2015-12-16 | 2016-04-06 | 苏州迪思伏新能源科技有限公司 | Preparation method for sphere-like lithium titanate electrode material |
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- 2016-08-15 CN CN201610668773.6A patent/CN106159250A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101630732A (en) * | 2009-07-27 | 2010-01-20 | 深圳市德方纳米科技有限公司 | Nanoscale lithium titanate compound and preparation method thereof |
| WO2012020998A2 (en) * | 2010-08-11 | 2012-02-16 | 주식회사 루트제이제이 | Method for preparing lithium titanium oxide, lithium titanium oxide prepared by same, and lithium secondary battery comprising the lithium titanium oxide |
| CN105406051A (en) * | 2014-09-16 | 2016-03-16 | 河南科隆新能源有限公司 | Composite lithium titanate preparation method |
| CN105470490A (en) * | 2015-12-16 | 2016-04-06 | 苏州迪思伏新能源科技有限公司 | Preparation method for sphere-like lithium titanate electrode material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092413A (en) * | 2019-05-09 | 2019-08-06 | 云南中烟工业有限责任公司 | A kind of method that spray drying-solid phase method prepares lithium titanate |
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