CN101580274B - Preparation method of high-purity one-dimensional Zn2Ti3O8 nano-material and application thereof in lithium battery - Google Patents

Preparation method of high-purity one-dimensional Zn2Ti3O8 nano-material and application thereof in lithium battery Download PDF

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CN101580274B
CN101580274B CN2009101120635A CN200910112063A CN101580274B CN 101580274 B CN101580274 B CN 101580274B CN 2009101120635 A CN2009101120635 A CN 2009101120635A CN 200910112063 A CN200910112063 A CN 200910112063A CN 101580274 B CN101580274 B CN 101580274B
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dimentional structure
nano material
preparation
lithium cell
nano
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CN101580274A (en
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魏明灯
洪振生
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Fuzhou University
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Fuzhou University
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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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention provides a preparation method of a high-purity one-dimensional Zn2Ti3O8 nano-material and application thereof in a lithium battery. The preparation method comprises the following steps: mixing a titanium dioxide powder with a caustic soda solution to react, washing the solution by a dilute hydrochloric acid, subsequently adding the solution in a water solution containing Zn(NH3)4<2+> for stirring, and finally roasting to obtain the one-dimensional Zn2Ti3O8 nano-material that is used for the lithium battery. The method for preparing the one-dimensional Zn2Ti3O8 nano-material has the advantages of low temperature, simple and convenient operation, low cost, high purity, excellent performance and capability of large-scale synthesis; and the one-dimensional Zn2Ti3O8 nano-material applied in the lithium battery has the advantages of high capability, good circulation performance and the like.

Description

High purity one-dimentional structure Zn 2Ti 3O 8Preparation of nanomaterials and the application in lithium cell thereof
Technical field
The invention belongs to technical field of lithium batteries, more specifically relate to a kind of high purity one-dimentional structure Zn 2Ti 3O 8Preparation of nanomaterials and the application in lithium cell thereof.
Background technology
The core of lithium ion battery is a lithium storage materials.At present, graphite is the negative material that is widely used in the commercialization lithium ion battery.But graphite embedding lithium current potential is low, and graphite surface may cause the deposition of metallic lithium in charge and discharge process, has certain potential safety hazard.Recently, spinel Li 4Ti 5O 12Owing to having excellent cycle performance and advantage such as nontoxic, safe becomes more promising negative material.But Li 4Ti 5O 12Theoretical capacity have only half of graphite, thereby the negative material of exploitation with good circulation performance and higher capacity remains the research emphasis in this field.
Summary of the invention
The purpose of this invention is to provide a kind of high purity one-dimentional structure Zn 2Ti 3O 8Preparation of nanomaterials and the application in lithium cell thereof, preparation Zn 2Ti 3O 8Nanometer material temperature is low, and is easy and simple to handle, cost is low, purity is high, excellent performance, can synthesize in a large number, adopts this Zn 2Ti 3O 8Nano material is applied in the lithium cell, has characteristics such as capacity height, good cycle.
High purity one-dimentional structure Zn 2Ti 3O 8Preparation of nanomaterials, it is characterized in that: described preparation method's step comprises: 2-5 gram titania powder and 20-50 ml concn are that 10-20 mol caustic soda soln mixes, at 100 ℃-140 ℃ reaction 20h, reactant after the dilute hydrochloric acid washing, is got the adding of 0.05-0.4 gram material and is contained Zn (NH again 3) 4 2+Ionic concn is to stir 24 hours under 60 ℃ in the 0.5-2 mol aqueous solution.At 450 ℃ of-650 ℃ of roasting 3h, prepare one-dimentional structure Zn then 2Ti 3O 8Nano material, this one-dimentional structure Zn 2Ti 3O 8Nano material is used for lithium cell.
Remarkable advantage of the present invention is: the present invention synthesizes high purity one-dimentional structure Zn first under lower temperature 2Ti 3O 8Nano material.With this high purity one-dimentional structure Zn 2Ti 3O 8Nano material is made lithium cell cathode material, finds that it has outstanding cycle performance and higher specific storage, it is applied in be applied in the lithium cell, has characteristics such as capacity height, good cycle.
Description of drawings
Fig. 1 is Zn of the present invention 2Ti 3O 8Nanometer rod see through electromicroscopic photograph.
Fig. 2 is the cycle characteristics figure of lithium cell of the present invention under different charging and discharging currents conditions.
Embodiment
Following according to the concrete elaboration of embodiment enforcement of the present invention.
Embodiment
Preparation method's step comprises: 2-5 gram titania powder and 20-50 ml concn are that the caustic soda soln of 10-20 mol mixes, and, get the 0.05-0.4 gram and add and contain Zn (NH again after the dilute hydrochloric acid washing at 100 ℃-140 ℃ reaction 20h reactants 3) 4 2+Ionic concn 0.5-2 mol Zn (NH 3) 4 2+60 ℃ were stirred 24 hours down in the aqueous solution; At 450 ℃ of-650 ℃ of roasting 3h, prepare one-dimentional structure Zn then 2Ti 3O 8Nano material.
The one-dimentional structure Zn for preparing according to present method 2Ti 3O 8The pattern parameter of nano material is: length is about the hundreds of nanometer to micron order, is formed by connecting by the particle about about tens nanometers of size, and concrete structure as shown in fig. 1.The described one-dimentional structure Zn that obtains fully 2Ti 3O 8The purity of nano material is: 70%-90%.
With one-dimentional structure Zn of the present invention 2Ti 3O 8Nano material is used for lithium cell.
Zn 2Ti 3O 8When nano material was used for lithium cell, this lithium cell assembling process comprised: lithium cell assembling: press mass ratio Zn 2Ti 3O 8: tetrafluoroethylene: acetylene black=mixed grinding after equably be coated in 0.25cm at 50: 10: 40 2Copper sheet on do positive pole, negative pole is a metallic lithium, ionogen is 1M LiClO 4EC+DEC+DMC solution, the volume ratio of EC in the described solution: DEC: DMC=1: 1: 1, the assembling process of above lithium cell all carries out in glove box.
The effect performance measurement: lithium cell is 0.3Ag in current density -1After 100 circulations, its specific storage still can reach 146mAh/g; Be 0.5Ag then in current density -1Again through after 100 circulations, its specific storage still reaches 123mAh/g down; And then return to 0.3Ag -1After 25 circulations, its specific storage still can reach 145mAh/g.Continuing in current density at last is 0.1Ag -1Through after 50 circulations, its specific storage still reaches 190mAh/g, as shown in Figure 2 down.These results show one-dimentional structure Zn 2Ti 3O 8Nano material is made lithium cell cathode material, and its cycle performance is very stable.

Claims (5)

1. high purity one-dimentional structure Zn 2Ti 3O 8Preparation of nanomaterials is characterized in that: described preparation method's step comprises: it is that the caustic soda soln of 10-20 mol mixes that 2-5 is restrained titania powder and 20-50 ml concn, at 100 ℃-140 ℃ reaction 20h; Reactant after the dilute hydrochloric acid washing, is got the adding of 0.05-0.4 gram material and is contained Zn (NH again 3) 4 2+Ionic concn be in the aqueous solution of 0.5-2 mol 60 ℃ stirred 24 hours down; At 450 ℃ of-650 ℃ of roasting 3h, prepare one-dimentional structure Zn then 2Ti 3O 8Nano material.
2. high purity one-dimentional structure Zn according to claim 1 2Ti 3O 8Preparation of nanomaterials is characterized in that: the one-dimentional structure Zn that described method prepares 2Ti 3O 8The pattern parameter of nano material is: length is that the hundreds of nanometer is to micron order, by the particle of the big or small tens nanometers one-dimentional structure that is formed by connecting; Preparation-obtained one-dimentional structure Zn 2Ti 3O 8The purity of nano material is: 70%-90%.
3. high purity one-dimentional structure Zn of method preparation as claimed in claim 1 or 2 2Ti 3O 8The purposes of nano material is characterized in that: described one-dimentional structure Zn 2Ti 3O 8Nano material is used for lithium cell.
4. high purity one-dimentional structure Zn according to claim 3 2Ti 3O 8The purposes of nano material is characterized in that: described Zn 2Ti 3O 8When nano material was used for lithium cell, this lithium cell assembling process comprised: lithium cell assembling: press mass ratio Zn 2Ti 3O 8: tetrafluoroethylene: acetylene black=mixed grinding after equably be coated in 0.25cm at 50: 10: 40 2Copper sheet on do positive pole, negative pole is a metallic lithium, ionogen is 1M LiClO 4EC+DEC+DMC solution, the volume ratio of EC in the described solution: DEC: DMC=1: 1: 1.
5. high purity one-dimentional structure Zn according to claim 4 2Ti 3O 8The purposes of nano material is characterized in that: the assembling process of described lithium cell all carries out in glove box.
CN2009101120635A 2009-06-25 2009-06-25 Preparation method of high-purity one-dimensional Zn2Ti3O8 nano-material and application thereof in lithium battery Expired - Fee Related CN101580274B (en)

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CN102050490A (en) * 2010-11-25 2011-05-11 福州大学 Synthesis of cathode material LiZnVO4 and application thereof in lithium battery
CN103801281B (en) * 2012-11-14 2016-01-20 上海纳米技术及应用国家工程研究中心有限公司 A kind of preparation method of zinc titanate quantum dot carried titanium dioxide nanobelt
CN103896328B (en) * 2014-03-13 2015-09-09 福建师范大学 Sub-zinc titanate nanometer sheet and its preparation method and application
CN106629830B (en) * 2017-01-10 2018-06-15 福州大学 A kind of zinc titanate nano-material and its application in perovskite solar cell
CN110581273B (en) * 2019-09-18 2021-04-13 东北大学秦皇岛分校 Zinc-position sodium-copper co-doped synergetic nitrogen-sulfur doped carbon-coated modified zinc titanate negative electrode material and preparation method and application thereof

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