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Method for fast preparing cobalt phosphide and product

A cobalt phosphide, fast technology, applied in phosphide and other directions, can solve the problems of cobalt phosphide that cannot control the particle size and composition, the preparation method is complicated, the reaction time is long, and the cost is low, the preparation process is simple, and the reaction time is short. Effect

Active Publication Date: 2018-11-13
NANJING UNIV OF POSTS & TELECOMM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The second is to use hydrogen to reduce metal phosphate. Since the bond energy between phosphorus and oxygen is strong, in order to destroy the bond between phosphorus and oxygen, the formation of metal-phosphorus bond can only occur at high temperature. However, this process is easy to form metal particles, while the formation of metal particles greatly enhances the adsorption of hydrogen by the metal, and at the same time overflows the phosphate, resulting in the reduction of phosphate to phosphide
The fourth is to use elemental phosphorus to prepare metal phosphides under hydrothermal conditions (140-200°C). The elemental phosphorus has white phosphorus, yellow phosphorus and red phosphorus as phosphorus sources, which may lead to the agglomeration of the prepared cobalt phosphide. No control over particle size and composition
[0004] The above methods of preparing cobalt phosphide by using different phosphorus sources not only have high cost, complicated preparation methods, long reaction time, but also release toxic gas

Method used

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  • Method for fast preparing cobalt phosphide and product
  • Method for fast preparing cobalt phosphide and product

Examples

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Effect test

Embodiment 1

[0034] A method for rapidly preparing cobalt phosphide, comprising the following steps:

[0035] Step (1), CoCl 2 ·6H 2 O and NaH 2 PO 2 ·H 2 The molar ratio of O is selected as 1:5, and 0.238g CoCl 2 ·6H 2 O and 0.530 g NaH 2 PO 2 ·H 2 O was added to an appropriate amount of deionized water and stirred on a magnetic stirrer to obtain a clear precursor solution;

[0036] Step (2), add an appropriate amount of surfactant to the precursor solution obtained in step (1), and continue stirring for 20 minutes to obtain a uniformly stirred precursor suspension;

[0037] Step (3), move the homogeneously stirred precursor suspension into a high-temperature reaction kettle, put the reaction kettle into an oven, react at 200°C for 3 hours, cool naturally to room temperature, and centrifugally clean the sediment in the reaction kettle , that is, to obtain the desired cobalt phosphide.

[0038] figure 1 It is the XRD pattern of the prepared cobalt phosphide, it can be seen from...

Embodiment 2

[0040] A method for rapidly preparing cobalt phosphide, comprising the following steps:

[0041] Step (1), CoCl 2 ·6H 2 O and NaH 2 PO 2 ·H 2 The molar ratio of O is selected as 1:10, and 0.238g CoCl 2 ·6H 2 O and 1.06 g NaH 2 PO 2 ·H 2 O was added to an appropriate amount of deionized water, and after stirring evenly on a magnetic stirrer, a clarified precursor solution was obtained;

[0042] Step (2), add an appropriate amount of surfactant to the precursor solution obtained in step (1), and continue to stir for 20 minutes;

[0043] Step (3), move the homogeneously stirred precursor suspension obtained in step (2) into a high-temperature reactor, put the reactor into an oven, react at 200°C for 3 hours, cool naturally to room temperature, and place the reactor The precipitate in the method was washed twice by centrifugation with absolute ethanol to obtain the desired product cobalt phosphide.

[0044] figure 2 b is the SEM spectrum of cobalt phosphide, in which ...

Embodiment 3

[0046] A method for rapidly preparing cobalt phosphide, comprising the following steps:

[0047] Step (1), CoCl 2 ·6H 2 O and NaH 2 PO 2 ·H 2 The molar ratio of O is selected as 1:15, and 0.238g CoCl 2 ·6H 2 O and 1.589 g NaH 2 PO 2 ·H 2 O was added to an appropriate amount of deionized water and stirred on a magnetic stirrer to obtain a clear precursor solution;

[0048] Step (2), add an appropriate amount of surfactant to the precursor solution obtained in step (1), and continue stirring for 20 minutes to obtain a uniformly stirred precursor suspension;

[0049] Step (3), move the homogeneously stirred precursor suspension in step (2) into a high-temperature reactor, put the reactor into an oven, react at 200°C for 3 hours, cool naturally to room temperature, and place the reactor in the The precipitate was washed twice by centrifugation with deionized water and absolute ethanol to obtain the desired product cobalt phosphide.

[0050] figure 2 c is the SEM spect...

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Abstract

The invention discloses a method for fast preparing cobalt phosphide and a product. Cobalt chloride CoCl2.6H2O cobalt source and sodium hypophosphite NaH2PO2.H2O phosphorus sources are used as raw materials; a proper proportion of raw materials are weighed and dissolved into deionized water for mixing to form precursor liquid; then, the precursor liquid and a surfactant are subjected to hydrothermal reaction for a period of time; through centrifugal cleaning, cobalt phosphide is obtained through preparation. The method for fast preparing cobalt phosphide and the product provided by the invention have the advantages that the ideal reaction time for preparing cobalt phosphide Co2P products by a one-step hydrothermal method is 3h; after the experiment reaction for 1h, expected products can occur, but the crystallinity degree is low; along with the reaction time prolonging; the crystal growth is complete; the particles are uniform; the preparation process is simple; the cost is low; the crystallinity degree is high; the reaction time is short; the repeatability is realized; the spherical structure cobalt phosphide formed by the polyhedrons can be fast obtained.

Description

technical field [0001] The invention relates to the technical field of preparation of functional materials, in particular to a method for rapidly preparing cobalt phosphide and a product thereof. Background technique [0002] Cobalt phosphide (Co 2 P) is an interstitial compound formed when phosphorus sources enter the transition metal cobalt lattice. Cobalt phosphide can be used in magnetism, lithium battery anode materials, hydrogenation catalysis and photocatalytic degradation. Cobalt phosphide is a semiconductor material with low band gap, high thermal stability, chemical stability, strong electrical conductivity and high-efficiency catalytic performance. And inexpensive transition metal phosphides. [0003] According to different sources of phosphorus, there are four methods for preparing cobalt phosphide. The first one uses trioctylphosphine (TOP) as a phosphorus source to synthesize phosphides, which can be obtained by thermal decomposition of metal phosphide comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08
CPCC01B25/08C01P2002/72C01P2004/03C01P2004/50
Inventor 李兴鳌贺艳娜张健崔任杰陈爱诗
Owner NANJING UNIV OF POSTS & TELECOMM
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