Method for preparing multi-shape controllable nano nikel-cobalt spinel oxide

A nano-cobalt and nickel acid technology, applied in chemical instruments and methods, nickel compounds, inorganic chemistry, etc., to achieve the effects of uniform morphology, easy availability and low price of materials, and stable size

Inactive Publication Date: 2014-08-27
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are many preparation methods of nickel cobaltate, such as spray pyrolysis, co-precipitation, polymer complex pyrolysis, electrospinning, template method and freeze-drying method, etc. Particles and nanowires, but currently the multi-level structure NiCo 2 o 4 The synthesis of

Method used

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  • Method for preparing multi-shape controllable nano nikel-cobalt spinel oxide
  • Method for preparing multi-shape controllable nano nikel-cobalt spinel oxide
  • Method for preparing multi-shape controllable nano nikel-cobalt spinel oxide

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Experimental program
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Effect test

Embodiment 1

[0035] An ultra-thin hierarchical structure NiCo 2 o 4 Synthetic method is characterized in that comprising the following steps:

[0036] Step S1a nickel nitrate Ni (NO 3 ) 2 ·6H 2 O and cobalt nitrate Co(NO 3 ) 2 ·6H 2 O is dissolved in absolute ethanol to form a solution A with a concentration of 0.6mmol / L according to the ratio of cobalt to nickel atoms;

[0037] In step S2a, oleylamine is dispersed into an ethanol solution at a volume fraction of 0.053 to form a solution B, and the solution B is mixed with the solution A at a volume ratio of B / A of 0.43 to obtain a mixed solution a;

[0038] In step S3a, after the mixed solution is fully stirred evenly, the mixed solution is moved into a dynamic reaction kettle, and after sealing, the H 2 , after the substitution H 2 When the pressure reaches 6bar, close the gas outlet valve of the cylinder;

[0039] In step S4a, adjust the stirring speed of the dynamic reactor to 400r / min, set the temperature at 150°C, and react...

Embodiment 2

[0045] An ultra-thin hierarchical structure NiCo 2 o 4 Synthetic method is characterized in that comprising the following steps:

[0046] Step S1b nickel nitrate Ni (NO 3 ) 2 ·6H 2 O and cobalt nitrate Co(NO 3 ) 2 ·6H 2 O is dissolved in dehydrated alcohol according to the ratio of the cobalt-nickel atomic ratio to form a solution A with a concentration of 0.1mmol / L;

[0047] In step S2b, oleylamine is dispersed into an ethanol solution at a volume fraction of 0.13 to form a solution B, and the solution B is mixed with the solution A at a volume ratio of B / A of 0.53 to obtain a mixed solution;

[0048] In step S3b, after the mixed solution is fully stirred evenly, the mixed solution is moved into a dynamic reaction kettle, and after sealing, the H 2 , after the substitution H 2 When the pressure reaches 15bar, close the cylinder outlet valve;

[0049] In step S4b, adjust the stirring speed of the dynamic reactor to 400r / min, set the temperature at 150°C, and react fo...

Embodiment 3

[0053] A kind of hollow sea urchin NiCo 2 o 4 Synthetic method is characterized in that comprising the following steps:

[0054] Step S1c nickel nitrate Ni (NO 3 ) 2 ·6H 2 O and cobalt nitrate Co(NO 3 ) 2 ·6H 2 O is dissolved in dehydrated alcohol according to the ratio of the cobalt-nickel atomic ratio to form a solution A with a concentration of 0.1mmol / L;

[0055] In step S2c, oleylamine is dispersed into an ethanol solution at a volume fraction of 0.13 to form a solution B, and the solution B is mixed with the solution A at a volume ratio of B / A of 0.53 to obtain a mixed solution;

[0056] In step S3c, after the mixed solution is fully stirred evenly, the mixed solution is moved into a dynamic reaction kettle, and after sealing, the H 2 , after the substitution H 2 When the pressure reaches 15bar, close the cylinder outlet valve;

[0057] In step S4c, adjust the stirring speed of the dynamic reactor to 400r / min, set the temperature at 150°C, and react for 10 hour...

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Abstract

The invention relates to a method for preparing multi-shape controllable nano nikel-cobalt spinel oxide. The method includes the steps that nickel nitrate and cobalt nitrate are dissolved in anhydrous ethanol according to the cobalt-nickel atom ratio to form a solution A; oleylamine is dispersed in an ethanol solution to form a solution B, and the solution B and the solution A are mixed to obtain a mixed solution; the mixed solution is fully and evenly stirred and moved into a dynamic reaction kettle, H2 is replaced in a sealed mode, pressure intensity of H2 is adjusted to 6-15 bar after replacement, and a steel cylinder air outlet valve is closed; the stirring speed of the dynamic reaction kettle is adjusted to 400 r/min, temperature is set to be 150 DEG C, and reaction is carried out for 10 h; a product is cleaned through ethanol and other nonpolar solvents respectively, centrifugal separation is carried out, and a sediment precursor is obtained through drying at the temperature of 60 DEG C; the temperature of the obtained sediment precursor rises in an air atmosphere at the speed of 10 DEG C/min, and the sediment precursor is heated to 200-400 DEG C and kept warm. According to the method, procedures are few, materials are easy to get and low in price, the procedures are safe, nikel-cobalt spinel oxide of different shapes can be obtained by changing a small condition in the procedures, and accordingly preparing of the controllable nano nikel-cobalt spinel oxide is achieved.

Description

technical field [0001] The invention relates to the field of synthesis of micro-nano materials, and mainly relates to a preparation method of multi-morphology controllable nano-nickel cobaltate. Background technique [0002] In recent years, the synthesis and application of porous materials with hierarchical structures, which can provide large active areas and shorten diffusion paths, have received extensive attention. At present, by controlling the surface of the basic unit of nanomaterials, the distance and orientation between the constituent units of the sub-nanostructure can be adjusted to further study the combination effect and synergy between the basic units. Therefore, the new phenomena and new properties of hierarchical nanostructures are conducive to the development of new mechanisms, which can lay the foundation for designing new materials with target properties. Spinel-type oxides have been extensively studied as promising anode materials due to their high catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00
Inventor 徐建张远邱会芸郭昌盛贺艳
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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