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A Surfactant-Assisted Hydrothermal Method for the Preparation of Bird's Nest-shaped CO3O4

A technology of surfactant and bird's nest is applied in the field of preparing Co3O4 with bird's nest shape by hydrothermal method, which can solve the problems such as no literature report in the background technology.

Inactive Publication Date: 2011-11-30
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the nest-shaped Co 3 o 4 There is no bibliographical information on the background technology of the preparation aspect

Method used

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  • A Surfactant-Assisted Hydrothermal Method for the Preparation of Bird's Nest-shaped CO3O4
  • A Surfactant-Assisted Hydrothermal Method for the Preparation of Bird's Nest-shaped CO3O4

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Embodiment 1: Under the condition of magnetic stirring, ammonia solution is slowly added dropwise to the solution containing 10mmol Co(NO 3 ) 2 In 30mL of transparent aqueous solution, the pH value is controlled between 9 and 10, so that the metal ions can be completely precipitated. Then add 1mL of ethylenediamine, and then transfer the mixture to a 50mL stainless steel reaction kettle lined with polytetrafluoroethylene (80% volume filling), and then put it in a constant temperature box at 140°C for 12h, and then place it at room temperature Cool down, filter the obtained turbid solution with suction, wash, dry (60°C, 12h), and grind evenly to obtain the precursor of the target product, which is then placed in a muffle furnace at a rate of 1°C / min in an air atmosphere Raise the temperature to 300°C and keep at 300°C for 4h to obtain single-phase cubic spinel Co 3 o 4 The powder is in the form of a relatively uniform bird's nest with a scaly surface, with a diameter ...

Embodiment 2

[0013] Embodiment 2: Under the condition of magnetic stirring, ammonia solution is slowly added dropwise to the solution containing 10mmol Co(NO 3 ) 2 In 30mL of transparent aqueous solution, the pH value is controlled between 9 and 10, so that the metal ions can be completely precipitated. Then add 1mL of dodecylamine, then transfer it to a 50mL stainless steel reactor lined with polytetrafluoroethylene (80% volume filling), and then put it in a constant temperature box at 120°C for 24h, and then place it at room temperature After cooling, the obtained turbid solution was suction-filtered, washed, dried (60°C, 12h), and ground uniformly to obtain the target product precursor, which was placed in a muffle furnace and heated to 300°C at a rate of 1°C / min in an air atmosphere. Keep at 300°C for 4h to obtain single-phase cubic spinel Co 3 o 4 The powder is in the shape of a relatively uniform bird's nest with a smooth surface and a diameter of about 42 μm. Its XRD spectrum is ...

Embodiment 3

[0014] Embodiment 3: Under the condition of magnetic stirring, the ammonia solution is slowly added dropwise to the solution containing 10mmol Co(NO 3 ) 2 In 30mL of transparent aqueous solution, the pH value is controlled between 9 and 10, so that the metal ions can be completely precipitated. Then add 1mL of ethylenediamine, then transfer it to a 50mL stainless steel reactor lined with polytetrafluoroethylene (80% volume filling), and then put it in a constant temperature box at 200°C for 12h, and then at room temperature After cooling, the obtained turbid solution was suction-filtered, washed, dried (60°C, 12h), and ground uniformly to obtain the target product precursor, which was placed in a muffle furnace and heated to 300°C at a rate of 1°C / min in an air atmosphere. Keep at 300°C for 4h to obtain single-phase cubic spinel Co 3 o 4 The powder is in the shape of a bird's nest with a scaly surface, and its diameter is about 30 μm. Its XRD spectrum is shown in figure 1 ...

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Abstract

The invention relates to an auxiliary hydro-thermal method for preparing a bird-nest-shaped Co3O4 surfactant, belonging to the technical field of functional materials. The method comprises the following steps of: under the stirring condition, dropwise adding ammonia water into a Co(NO3)2 aqueous solution with the concentration of 0.33-0.34mol / L, controlling the pH value to be 9-10, completely precipitating metal ions, adding ethylene diamine (the mol ratio of ethylene diamine to Co(NO3)2 is 2:3) or dodecyl amine (the mol ratio of dodecyl amine to Co(NO3)2 is 43: 100), transferring the solution into a stainless steel reaction kettle with the lining of 50ml of polytetrafluoroethylene and filling volume of 80%, insulating for 24 hours at the temperature of 120 DEG C or insulating for 12 hours at the temperature of 140 or 200 DEG C, cooling to room temperature, carrying out suction filtering, washing, drying for 12 hours at the temperature of 60 DEG C, grinding, and rapidly warming to 300DEG C in the air at the rate of 1 DEG C / min and maintaining the temperature for 4 hours. A sample is a bird-nest-shaped structure with a platelike surface.

Description

technical field [0001] The invention relates to a Co 3 o 4 The preparation method, specifically relates to the preparation of a bird's nest-shaped Co 3 o 4 , belonging to the technical field of functional materials. Background technique [0002] co 3 o 4 It is an important functional material widely used in electrochromic devices, ceramic pigments, catalysis, solid-state sensors, magnetism, solar absorption devices, and energy storage (interlayer compounds for lithium-ion rechargeable batteries). Therefore, for Co 3 o 4 A lot of research work has been done on the synthetic methods. Co has been synthesized with various morphologies 3 o 4 , such as hollow nanospheres (S.A.Makhlouf, J.Magn.Mater., 2002, 246:184-190), fibrous (B.B.Lakshmi, et al., Chem.Mater., 1997, 9:2544-2550), Nanorods, nanotubes, nanostructure films (A. Gulino, et al., Chem. Mater., 2003, 15: 3748-3752), etc. Nanowire-like Co 3 o 4 porous Al 2 o 3 Or virus (K.T.Nam, et al., Science, 2006, 312...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 戴洪兴王芳白广梅邓积光吉科猛刘雨溪高宝族
Owner BEIJING UNIV OF TECH
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