CN101920989A - Preparation method of novel spinel titanate nano material and application thereof in lithium battery - Google Patents
Preparation method of novel spinel titanate nano material and application thereof in lithium battery Download PDFInfo
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- CN101920989A CN101920989A CN2010102358855A CN201010235885A CN101920989A CN 101920989 A CN101920989 A CN 101920989A CN 2010102358855 A CN2010102358855 A CN 2010102358855A CN 201010235885 A CN201010235885 A CN 201010235885A CN 101920989 A CN101920989 A CN 101920989A
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- spinel titanate
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- 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
Abstract
The invention relates to a preparation method of a novel spinel titanate nano material and an application thereof in a lithium battery. The preparation method is characterized by comprising the following steps: (1) mixing 0.5-1.5g of titanium dioxide powder and 40-50ml of caustic soda solution with the concentration of 10-20mol/L, and reacting for 48-96h under the temperature of 160-200 DEG C; and (2) after washing the reactants by diluted hydrochloric acid, taking 0.1-0.5g of the reactants, mixing the reactants with lithium hydroxide as well as a corresponding metal acetate or a metal oxide in 10-35ml of absolute ethyl alcohol based on a certain mole ratio, stirring for 20-72h, and baking for 3-7h at the temperature of 550-850 DEG C to prepare the spinel titanate nano material. The preparation method has the advantages of simple and convenient operation, low cost and easily mass synthesis; and the prepared spinel titanate nano material has high purity and favorable performance, and when being used as a lithium battery anode material, the nano material is favor for improving circulation stability, specific capacity and charge-discharge speed of the lithium battery.
Description
Technical field
The present invention relates to a kind of preparation method of novel spinel titanate nano material and the application in lithium cell thereof.
Background technology
Significant advantage, the current fields such as mobile electronic device, national defense industry, electromobile that have been widely used in such as lithium ion battery has high-voltage, heavy body, have extended cycle life.Wherein, because the needs of the energy and environment protection, electromobile has become industry of greatest concern in the current new energy field.Thereby developing high performance lithium-ion-power cell has become one of the most popular in recent years research field.Current, power battery anode materials such as spinel lithium manganate, iron lithium phosphate are by extensive studies and obtained bigger progress.Yet, but less relatively for the research of cathode material of lithium-ion power battery.And there is certain potential safety hazard in traditional graphite surperficial deposition that may cause metallic lithium in charge and discharge process.Thereby exploitation has the fast charging and discharging ability, cyclicity is good, specific storage is high negative material has crucial meaning.
The relevant patent report that the preparation and the application in lithium cell thereof of this kind novel spinel titanate nano wire, nanoparticle are not also arranged at present.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of novel spinel titanate nano material and the application method in lithium cell thereof, this preparation method is easy and simple to handle, cost is low, be convenient to a large amount of synthetic, the novel spinel titanate nano material purity height for preparing, performance is good, and it is used as the Anode of lithium cell material, helps improving cyclical stability, the specific storage of lithium cell and discharges and recharges speed.
For achieving the above object, the invention provides a kind of preparation method of novel spinel titanate nano material, it is characterized in that: this method comprises following steps:
(1) be that the caustic soda soln of (10 ~ 20) mol mixes with (0.5 ~ 1.5) gram titania powder and (40 ~ 50) ml concn, under the temperature of (160 ~ 200) ℃, react (48 ~ 96) hour;
(2) reactant is after the dilute hydrochloric acid washing, get (0.1 ~ 0.5) gram, be mixed in the dehydrated alcohol of (10 ~ 35) milliliter by certain mol proportion and lithium hydroxide and corresponding metal acetate or metal oxide, after stirring (20 ~ 72) hour, at the roasting temperature (3 ~ 7) of (550 ~ 850) ℃ hour, prepare spinel titanate nano material again.
The present invention also provides a kind of application of adopting as the novel spinel titanate nano material of method for preparing, it is characterized in that: described spinel Li
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano material is applied in the lithium cell as the Anode of lithium cell material, and the assemble method of this lithium cell is: press mass ratio Li
2MTi
3O
8: polyvinylidene difluoride (PVDF): be coated in 0.25 cm equably behind acetylene black=70 ~ 75:5 ~ 10:15 ~ 20 mixed grindings
2Copper sheet on do positive pole, negative pole is a metallic lithium, ionogen is 1M LiClO
4EC+DMC+EMC, the volume ratio of EC:DMC:EMC is 1:1:1 in the described solution.
The invention has the beneficial effects as follows the present invention under lower temperature, synthesize the spinel Li of high purity (more than 90%) first
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano material, and preparation method of the present invention is easy and simple to handle, and cost is low, is convenient to a large amount of synthetic of novel spinel titanate nano material.And the novel spinel titanate nano material purity height for preparing, performance is good, and it is used as the Anode of lithium cell material, helps improving cyclical stability, the specific storage of lithium cell and discharges and recharges speed, therefore, has wide market application prospect.
The present invention is described in further detail below in conjunction with drawings and the specific embodiments.
Description of drawings
Fig. 1 is the preparation flow figure of spinel titanate nano material of the present invention.
Fig. 2 is spinel titanate nano wire cycle performance test result figure of the present invention.
Embodiment
The preparation method of novel spinel titanate nano material of the present invention, as shown in Figure 1, carry out as follows:
(1) be that the caustic soda soln of (10 ~ 20) mol mixes with (0.5 ~ 1.5) gram titania powder and (40 ~ 50) ml concn, under the temperature of (160 ~ 200) ℃, react (48 ~ 96) hour;
(2) reactant is after the dilute hydrochloric acid washing, get (0.1 ~ 0.5) gram, be mixed in the dehydrated alcohol of (10 ~ 35) milliliter by certain mol proportion and lithium hydroxide and corresponding metal acetate or metal oxide, after stirring (20 ~ 72) hour, at the roasting temperature (3 ~ 7) of (550 ~ 850) ℃ hour, prepare spinel titanate nano material again.In this step, during preparation spinel titanate nano wire, need to adopt metal acetate salt to mix, and during preparation spinel titanate nanoparticle, need mix with described reactant by the employing metal oxide with described reactant.
The chemical formula of above-mentioned spinel titanate nano material is Li
2MTi
3O
8, wherein M represents a kind of metal, according to the difference of metallic element in used metal acetate salt of step (2) or the metal oxide, M is a kind of among Metal Zn, Co, Mg or the Cu.
Adopt application, described spinel Li as the novel spinel titanate nano material of method for preparing
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano material is applied in the lithium cell as the Anode of lithium cell material.Described spinel Li
2MTi
3O
8(M=Zn, Co, Mg, when Cu) nano material was applied in the lithium cell, the assemble method of this lithium cell was: press mass ratio Li
2MTi
3O
8: polyvinylidene difluoride (PVDF): be coated in 0.25 cm equably behind acetylene black=70 ~ 75:5 ~ 10:15 ~ 20 mixed grindings
2Copper sheet on do positive pole, negative pole is a metallic lithium, ionogen is 1M LiClO
4EC+DMC+EMC, the volume ratio of EC:DMC:EMC is 1:1:1 in the described solution.And in this process, all assemblings are all carried out in glove box.
The present invention synthesizes high purity (more than 90%) spinel Li first under lower temperature
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano wire, its length is about the hundreds of nanometer to several microns, and diameter is tens to nanometers up to a hundred.In addition, the present invention has also successfully prepared Li
2MTi
3O
8(M=Zn, Co, Mg, Cu) nanoparticle, its particle diameter are about tens to nanometers up to a hundred.With this high purity Li
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano wire or nanoparticle be as the Anode of lithium cell material, and the result shows that they have outstanding cyclical stability, higher specific storage and superior fast charging and discharging performance.Wherein, Li
2ZnTi
3O
8Nano wire is 0.1 Ag in current density
-1After 90 circulations, its specific storage still can reach 240 mAhg
-1In current density up to 3.2 Ag
-1The time (just finish once discharge and recharge) less than 5 minutes, its specific storage still can be stabilized in 129 mAhg
-1Table 1 is depicted as Li
2MTi
3O
8(M=Zn, Co, Mg, Cu) nanowire electrochemical test result.
Table 1 Li
2MTi
3O
8(M=Zn, Co, Mg, Cu) nanowire electrochemical test result
| ? | Li 2ZnTi 3O 8 | Li 2CoTi 3O 8 | Li 2MgTi 3O 8 | Li 2CuTi 3O 8 |
| Specific storage (mAhg -1） | 240 | 220 | 165 | 160 |
| Capability retention (%) | 95 | 95 | 95 | 90 |
More than be preferred embodiment of the present invention, all changes of doing according to technical solution of the present invention when the function that is produced does not exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.
Claims (5)
1. the preparation method of a novel spinel titanate nano material, it is characterized in that: this method comprises following steps:
(1) be that the caustic soda soln of (10 ~ 20) mol mixes with (0.5 ~ 1.5) gram titania powder and (40 ~ 50) ml concn, under the temperature of (160 ~ 200) ℃, react (48 ~ 96) hour;
(2) reactant is after the dilute hydrochloric acid washing, get (0.1 ~ 0.5) gram, be mixed in the dehydrated alcohol of (10 ~ 35) milliliter by certain mol proportion and lithium hydroxide and corresponding metal acetate or metal oxide, after stirring (20 ~ 72) hour, at the roasting temperature (3 ~ 7) of (550 ~ 850) ℃ hour, prepare spinel titanate nano material again.
2. the preparation method of novel spinel titanate nano material according to claim 1, it is characterized in that: during preparation spinel titanate nano wire, in step (2), adopt metal acetate salt to mix with described reactant, and during preparation spinel titanate nanoparticle, the employing metal oxide mixes with described reactant in step (2).
3. the preparation method of novel spinel titanate nano material according to claim 1 and 2, it is characterized in that: the chemical formula of described spinel titanate nano material is Li
2MTi
3O
8, wherein M represents a kind of metal, according to the difference of metallic element in used metal acetate salt of step (2) or the metal oxide, M is a kind of among Metal Zn, Co, Mg or the Cu.
4. an employing is characterized in that: described spinel Li as the application of the novel spinel titanate nano material of method preparation as described in the claim 3
2MTi
3O
8(M=Zn, Co, Mg, Cu) nano material is applied in the lithium cell as the Anode of lithium cell material.
5. the application of novel spinel titanate nano material according to claim 4 is characterized in that: described spinel Li
2MTi
3O
8(M=Zn, Co, Mg, when Cu) nano material was applied in the lithium cell, the assemble method of this lithium cell was: press mass ratio Li
2MTi
3O
8: polyvinylidene difluoride (PVDF): be coated in 0.25 cm equably behind acetylene black=70 ~ 75:5 ~ 10:15 ~ 20 mixed grindings
2Copper sheet on do positive pole, negative pole is a metallic lithium, ionogen is 1M LiClO
4EC+DMC+EMC, the volume ratio of EC:DMC:EMC is 1:1:1 in the described solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320825A (en) * | 2011-08-16 | 2012-01-18 | 广西新未来信息产业股份有限公司 | Low-temperature sintered microwave dielectric ceramic and sintering method thereof |
| CN103715408A (en) * | 2013-12-13 | 2014-04-09 | 天津大学 | Sol-gel preparation method of lithium zinc titanate as lithium ion battery cathode material |
| CN103762350A (en) * | 2014-02-19 | 2014-04-30 | 厦门大学 | Titanium-containing anode material for lithium electrode and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486488A (en) * | 2009-01-20 | 2009-07-22 | 河南大学 | Preparation of nano spinelle lithium titanate |
-
2010
- 2010-07-26 CN CN2010102358855A patent/CN101920989A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486488A (en) * | 2009-01-20 | 2009-07-22 | 河南大学 | Preparation of nano spinelle lithium titanate |
Non-Patent Citations (2)
| Title |
|---|
| 《Electrochemistry Communications》 20100327 Zhensheng Hong et al. Li2ZnTi3O8 nanorods: A new anode material for lithium-ion battery 720-723 1-5 第12卷, 2 * |
| 《Materials chemistry and physics》 20031231 M.S.C.Camara et al. Synthesis and characterization of Li2ZnTi3O8 spinel using the modified polymeric precursor method 68-72 1-5 第82卷, 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320825A (en) * | 2011-08-16 | 2012-01-18 | 广西新未来信息产业股份有限公司 | Low-temperature sintered microwave dielectric ceramic and sintering method thereof |
| CN102320825B (en) * | 2011-08-16 | 2013-04-10 | 广西新未来信息产业股份有限公司 | Low-temperature sintered microwave dielectric ceramic and sintering method thereof |
| CN103715408A (en) * | 2013-12-13 | 2014-04-09 | 天津大学 | Sol-gel preparation method of lithium zinc titanate as lithium ion battery cathode material |
| CN103715408B (en) * | 2013-12-13 | 2016-03-16 | 天津大学 | The sol-gel process for preparing of lithium ion battery negative material zinc titanate lithium |
| CN103762350A (en) * | 2014-02-19 | 2014-04-30 | 厦门大学 | Titanium-containing anode material for lithium electrode and preparation method thereof |
| CN103762350B (en) * | 2014-02-19 | 2016-06-15 | 苏州德尔石墨烯产业投资基金管理有限公司 | A kind of titanium system negative material for lithium electricity and preparation method thereof |
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Application publication date: 20101222 |