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A kind of preparation method and use of titanium cobalt spinel

A technology of spinel and cobalt titanate is applied in the field of preparation of titanium cobalt spinel, which can solve the problems of difficulty in controlling particle morphology and size, inability to obtain regular morphology, and restricting the application of materials. Excellent cycle stability, easy operation effect

Active Publication Date: 2017-06-20
CHINA UNIV OF MINING & TECH
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  • Description
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Problems solved by technology

The traditional preparation method of titanium-cobalt spinel mainly adopts the solid-phase synthesis method, the reaction temperature is high, the time is long, the shape and size of the particles are difficult to control, and the regular shape cannot be obtained.
However, so far, the preparation method of titanium-cobalt spinel with good chemical composition uniformity, high purity and regular microstructure has not been reported, especially the titanium-cobalt spinel material with special morphology is still blank. greatly restricts the further application of the material

Method used

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  • A kind of preparation method and use of titanium cobalt spinel
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  • A kind of preparation method and use of titanium cobalt spinel

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preparation example Construction

[0031] Preparation method, it comprises the following steps:

[0032] (1) The cobalt source is divalent cobalt salt, selected from hydrated cobalt chloride (CoCl 2 ·6H 2 O), cobalt oxalate hydrate (CoC 2 o 4 2H 2 O), hydrated cobalt acetate (C 4 h 6 o 4 ·Co·4H 2 O) or cobalt nitrate hydrate (Co(NO 3 ) 2 ·6H 2 O);

[0033] The titanium source is selected from titanium dioxide (TiO 2 ), butyl titanate (C 16 h 36 o 4 Ti) or hydrated titanium sulfate (Ti(SO 4 ) 2 9H 2 O);

[0034] Solution 1 is prepared by adding titanium source to 0.5-2 mol / L lye; adding cobalt source to a solution with a mass ratio of sugar adjuvant: amine adjuvant = 2:1 to obtain solution 2. Mix solution 1 and solution 2 according to the molar ratio (1-5) of cobalt source and titanium source: 1 and stir evenly;

[0035] (2) Move the mixed material obtained in step (1) into a closed reactor at 100-250°C, react for 8-40 hours, cool naturally to room temperature, and then separate and purify to...

Embodiment 1

[0046] Example 1: Preparation and structural characterization of titanium-cobalt spinel nano-octahedron

[0047] Take 0.06g TiO 2 and 1.2g NaOH are put into the container and add 30ml deionized water to be mixed with suspension 1, get 0.3 g cobalt chloride hydrate (CoCl 2 ·6H 2 O), 0.1 g glucose and 0.05 g hydroxylamine chloride (H 3 NO·HCl) into a container and add 10ml of distilled water to make solution 2; mix and stir the suspension 1 and solution 2 evenly and transfer the mixed material to a closed pressure-resistant reaction vessel for reaction at 200°C 48 hours. Then cool to room temperature, open the airtight reaction vessel, and filter with Buchner funnel, wash with deionized water and absolute ethanol repeatedly to obtain a dark green powder product. The product was identified as cubic titanium-cobalt spinel Co 2 TiO 4 ( figure 1 ), which matches the JCPDS card standard value No. 39-1410, and no other impurity peaks appear.

[0048] figure 1 It is the powder...

Embodiment 2

[0052] Embodiment 2: get 0.06g TiO 2 and 1.2g NaOH are put into container and add 30ml deionized water and be mixed with suspension 1, get 0.31 g hydrated cobalt acetate (C 4 h 6 o 4 ·Co·4H 2 O), 0.2 g glucose and 0.1 g hydroxylamine chloride (H 3 NO·HCl) into a container and add 10ml of distilled water to prepare solution 2; mix and stir the suspension 1 and solution 2 evenly, transfer the mixed material to a closed pressure-resistant reaction vessel, and react at 180°C 48 hours. Then cool to room temperature, open the airtight reaction vessel, and repeatedly centrifuge and wash with deionized water and absolute ethanol to obtain a dark green powder product.

[0053] The obtained ultrafine powder is cubic titanium-cobalt spinel (JCPDS No. 39-1410), with good crystallinity; the product is composed of nano-octahedrons with an average particle size of about 170 nm.

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Abstract

A preparation method and application of titanium-cobalt spinel belongs to preparation methods and applications of transition-metal spinel, and specifically is a preparation method for a titanium-cobalt spinel (Co2TiO4) octahedral-nanostructure material and an application of the titanium-cobalt spinel (Co2TiO4) octahedral-nanostructure material to a negative electrode material of a lithium ion battery. A mild liquid phase synthesis technique is utilized to prepare a cobalt titanate nanostructure, and parameters in a reaction process are adjusted and controlled, so that the titanium-cobalt spinel octahedral-nanostructure material is compounded conveniently in low cost and is applied as the negative electrode material of the lithium ion battery. The preparation method comprises the steps of: respectively preparing solutions by utilizing a titanium source and a cobalt source, mixing the prepared solutions according to a molar ratio of (1-5) : 1, stirring the mixed solution uniformly, and putting the uniformly stirred solution in a closed pressure-resistant vessel to react for 8-40 hours at 100-250 DEG C, wherein an alkali additive is added to the titanium-source preparation solution, and a saccharide additive and an amine additive are added to the cobalt-source preparation solution. According to the preparation method, the raw materials are easy to obtain, a synthesis method is simple, and the controllability of operation steps is high; the obtained titanium-cobalt spinel has high purity and uniform particle size, and expanded production is easy. If the titanium-cobalt spinel octahedral-nanostructure material is taken as the negative electrode material of the lithium ion battery, the electrochemical performance is excellent.

Description

technical field [0001] The invention relates to a preparation method and application of a transition metal spinel, in particular to a preparation method and application of a titanium-cobalt spinel. Background technique [0002] As a member of the field of inorganic functional materials, transition metal spinel nanomaterials have important properties such as size effect, quantum effect, and surface effect, and are widely used in optics (Chem. Eur. J., 2007, 13, 746), Magnetic (J.Am. Chem. Soc., 2008, 130, 13490), catalysis (Chem. Commun., 2009, 1565), electrochemical energy storage (J. Mater. Chem. A, 2013, 1, 9024), etc. The field has a wide range of applications. Since the particle size and morphology of the material have a serious impact on the physical and chemical properties of the material, it is necessary to control the synthesis of the material purposefully to obtain the desired excellent performance. [0003] Inverse spinel titanium cobalt green (Co 2 TiO 4 ) due...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/525H01M10/0525
CPCH01M4/525H01M10/0525Y02E60/10
Inventor 邢政马光耀鞠治成赵宇龙
Owner CHINA UNIV OF MINING & TECH
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