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Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof

A three-dimensional porous, sea urchin-like technology, applied in the field of materials science, can solve the problems of decreased electrocatalytic activity, easy aggregation of nanoparticles, and reduced active sites, and achieves the effect of simple steps, easy to obtain reagents, and favorable retention

Active Publication Date: 2015-11-04
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these cobalt phosphide nanowires and nanoparticles are easy to agglomerate during use, resulting in a sharp decrease in active sites, a decrease in electrocatalytic activity, and poor stability, so they are not suitable for practical applications.

Method used

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  • Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof
  • Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof
  • Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof

Examples

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preparation example Construction

[0039] In some more specific embodiments, the preparation method includes the following steps:

[0040] Ⅰ. Mix cobalt salt with neutral polar solvent, and then ultrasonically disperse evenly;

[0041] Ⅱ. After adding the amino compound to the mixed solution treated in step I and mixing and dispersing evenly, react at 100-150° C. for 1-24 hours;

[0042] Ⅲ. After the reaction is over, centrifuge to separate the hydrothermal reaction product obtained in step Ⅱ, then wash the product, and dry the product at 60°C;

[0043] IV. Annealing the product obtained in step III with hypophosphite at 200-400° C. for 2-10 hours to obtain the target product.

[0044] The aforementioned cobalt salts, amino compounds, hypophosphite salts, and neutral polar solvents can be selected from, but not limited to, the types listed above.

[0045] Further, in a typical embodiment, the preparation method may include: first dissolving cobalt nitrate in water, adding urea and ultrasonically dispersing it...

Embodiment 1

[0051] Example 1 Dissolve 0.5mmol of cobalt nitrate in 30mL of water, ultrasonically disperse evenly, then add 1.5mmol of urea, continue stirring for 30 minutes, then transfer the solution to a 50mL reactor, react at 120°C for 12 hours, cool down, and centrifuge Collect the product three-dimensional sea urchin-like hydrated basic cobalt carbonate precursor (for its morphology, please refer to Figure 1a-Figure 1b ), and annealed with 0.25 g of sodium hypophosphite at 300 ° C for 2 hours under the protection of nitrogen to obtain a three-dimensional porous sea urchin-like cobalt phosphide.

[0052] From Figure 2a-Figure 2b It can be seen from the figure that the cobalt phosphide product of this example is uniform in size, about 5 μm in diameter, and has a three-dimensional porous sea urchin-like structure. see again Figure 3a-Figure 3b , the product was determined to be orthorhombic cobalt phosphide by X-ray powder diffraction.

[0053] Dissolve 5 mg of cobalt phosphide and...

Embodiment 2

[0054] Example 2 Dissolve 1mmol of cobalt chloride in 30mL of ethanol, and disperse evenly by ultrasonication. Then, add 5mmol of urea, continue stirring for 30 minutes, then transfer the solution to a 50mL reactor, and react at 100°C for 10 hours. The product was collected and annealed with 0.25 g of potassium hypophosphite at 400° C. for 4 hours under the protection of argon to obtain a three-dimensional porous sea urchin-like cobalt phosphide.

[0055] In addition, the inventors of this case also used the other raw materials and other process conditions listed above to replace the various raw materials and corresponding process conditions in Examples 1-2 and carried out corresponding experiments. The obtained three-dimensional porous sea urchin-like cobalt phosphide Appearance, performance etc. are also comparatively ideal, basically similar to the product of embodiment 1-2.

[0056] The present invention first prepares three-dimensional sea urchin-shaped hydrated basic cob...

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Abstract

The invention discloses three-dimensional porous urchin-like cobalt phosphide as well as a preparation method and an application thereof. The preparation method comprises the steps of: uniformly mixing a cobalt salt and an amino compound in a neutral-polarity solvent to have hydrothermal reaction to prepare a three-dimensional urchin-like hydrated basic cobalt carbonate precursor mainly formed by assembly of nanowires; and annealing the hydrated basic cobalt carbonate precursor and hypophosphite at a high temperature to obtain the three-dimensional urchin-like cobalt phosphide. By preparing the three-dimensional urchin-like hydrated basic cobalt carbonate precursor by a simple hydrothermal process and obtaining the three-dimensional urchin-like cobalt phosphide through high temperature phosphorization, not only is the process simple and controllable, the source of raw material wide and the cost low, but also the yield is relatively high, and the mass production is realized. The prepared product is uniform in size, has an urchin-like porous structure, maintains more catalytic active sites, has high activity and excellent stability and is wide in application prospect in the field of electric catalysis.

Description

technical field [0001] The invention relates to a metal phosphide material and a preparation method thereof, in particular to a three-dimensional porous sea urchin-like cobalt phosphide, a preparation method and application thereof, and belongs to the field of material science. Background technique [0002] With the increasing energy crisis and environmental pollution caused by fossil energy, people urgently need to find a new energy containing energy that is clean, efficient and abundant. Hydrogen is an ideal new energetic energy. Hydrogen production by electrolysis of water is one of the most concerned hydrogen production methods at present. Its core technology is catalyst, and the most ideal catalyst is known to be platinum. However, due to the low reserve and high price of platinum, its application is greatly limited. [0003] At present, cobalt phosphide is considered to be one of the most likely substitutes for platinum catalysts due to its abundant reserves and excel...

Claims

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Application Information

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IPC IPC(8): C01B25/08C01B3/04B01J27/185
CPCY02E60/36
Inventor 王强斌杨红超
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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