Preparation method of regularly octahedral cobalt oxide micro-nano-particle material

A technology of micro-nano particles and regular octahedrons, applied in the direction of cobalt oxide/cobalt hydroxide, etc., to achieve the effects of low energy consumption, simple process flow, and high electrochemical stability

Inactive Publication Date: 2018-03-23
SHAANXI UNIV OF SCI & TECH
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  • Description
  • Claims
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Problems solved by technology

However, it is worth pointing out that no CoCl 2 ·6H 2 O and CO(NH 2 ) 2 As a raw material hydrothermal reaction system, the preparation of octahedral Co 3 o 4 Literature reports on micro-nano materials

Method used

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  • Preparation method of regularly octahedral cobalt oxide micro-nano-particle material
  • Preparation method of regularly octahedral cobalt oxide micro-nano-particle material
  • Preparation method of regularly octahedral cobalt oxide micro-nano-particle material

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preparation example Construction

[0030] The present invention octahedral Co 3 o 4 The preparation method of micro-nano particle material, comprises the following steps:

[0031] S1. Weigh CoCl 2 ·6H 2 O was added to deionized water, where CoCl 2 ·6H 2 O and H 2 The mass ratio of O is 1:80.00~106.34, ultrasonically dispersed for 20~30min to form a uniform wine red solution;

[0032] S2. Weigh CO(NH 2 ) 2 Join in the solution prepared in step S1, wherein, CO(NH 2 ) 2 with CoCl 2 ·6H 2 The mass ratio of O is 4:5, ultrasonically dispersed for 20-30 minutes to obtain a uniform solution;

[0033] S3. Transfer the solution obtained in step S2 to a stainless steel autoclave lined with polytetrafluoroethylene, with a filling ratio of 50-60%, seal it, react at 150° C. for 4-12 hours, collect the precipitate, wash it, and vacuum-dry it. Get a pink precursor;

[0034] Preferably, the inner volume of the stainless steel autoclave is 32.8-36.4mL.

[0035] S4. Transfer the precursor obtained in step S3 to a m...

Embodiment 1

[0038] Weigh 0.2050g of CoCl 2 ·6H 2 O, added to 16.4 mL of deionized water, CoCl 2 ·6H 2 O and H 2 The mass ratio of O was 1:80.00, and ultrasonically dispersed for 20 minutes to form a uniform wine-red solution.

[0039] Subsequently, weigh 0.1640g of CO(NH 2 ) 2 Add to the above solution, ultrasonically disperse for 20min.

[0040] The above solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave with a volume of 32.8mL, the filling ratio was 50%, sealed, and reacted at 140°C for 4h, the precipitate was collected, washed and dried, and a pink precursor was obtained.

[0041] The above precursor was transferred to a muffle furnace, and the temperature was raised to 400 °C at a rate of 5 °C / min, and kept for 4 h.

[0042] Subsequently, naturally cooled to room temperature, the octahedral Co 3 o 4 micro-nanomaterials, such as figure 1 shown.

Embodiment 2

[0044] Weigh 0.2050g of CoCl 2 ·6H 2 O was added to 16.4 mL of deionized water, CoCl 2 ·6H 2 O and H 2 The mass ratio of O was 1:80.00, and ultrasonically dispersed for 25 minutes to form a uniform wine-red solution.

[0045] Subsequently, weigh 0.1640g of CO(NH 2 ) 2 Add to the above solution, ultrasonically disperse for 25min.

[0046] The above solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave with a volume of 32.8mL, sealed, and reacted at 150°C for 6h, and the precipitate was collected, washed and dried to obtain a pink precursor.

[0047] The above-mentioned pink precursor was transferred to a muffle furnace, and the temperature was raised to 400 °C at a rate of 5 °C / min, and kept for 4 h.

[0048] Subsequently, naturally cooled to room temperature, the octahedral Co 3 o 4 micro-nanomaterials, such as figure 2 shown.

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Abstract

The invention discloses a preparation method of a regularly octahedral cobalt oxide micro-nano-particle material. CoCl2.6H2O is taken as a raw material, CO(NH2)2 is taken as a precipitant, deionized water is taken as a solvent, a rod-like precursor grows into a micro-rod formed by octahedral Co3O4 firstly and then the micro-rod grows gradually until regularly octahedral particles are formed. According to the method, CoCl2.6H2O and CO(NH2)2 as two simple raw materials are adopted under a mild hydrothermal condition, the deionized water is taken as the solvent, the rod-like precursor grows intothe micro-rod formed by octahedral Co3O4 firstly and then the micro-rod grows gradually until the regularly octahedral particles are formed, so that regularly octahedral Co3O4 and the micro-rod structure formed by regularly octahedral Co3O4 are prepared in a controllable manner, and the material not only has higher electrochemical stability, but also shows excellent electrochemical sensing property on H2O2.

Description

technical field [0001] The invention belongs to the technical field of preparation of micro-nano materials, in particular to a regular octahedral Co 3 o 4 Preparation method of micro-nano particle material. Background technique [0002] As a transition metal oxide semiconductor material, Co 3 o 4 With a variety of morphological characteristics and excellent magnetic properties, photocatalysis and energy storage properties, it has attractive prospects in the fields of catalysts, lithium-ion batteries, supercapacitors, gas sensor sensitive components and electrochemical sensors. One of the hotspots of nanomaterials research. co 3 o 4 There are many preparation methods, commonly used chemical spray pyrolysis method, chemical vapor precipitation method, liquid phase precipitation method, sol-gel method and hydrothermal method. Among them, the hydrothermal method has the advantages of mild hydrothermal reaction conditions, high product purity, complete grain development, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
CPCC01G51/04C01P2002/72C01P2004/03C01P2004/41
Inventor 张新孟张艺华于成龙伍媛婷王秀峰刘长青
Owner SHAANXI UNIV OF SCI & TECH
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