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Preparation method of transition metal phosphide with good morphology

A transition metal and phosphide technology, applied in phosphide and other directions, can solve the problems of inability to prepare phosphide, poor catalytic activity of the product, mixed crystal phase of the product, etc., and achieve the effect of being suitable for large-scale production, low cost and good crystalline performance

Inactive Publication Date: 2015-03-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] b), hydrothermal synthesis cannot prepare supported phosphides, and the obtained product has poor catalytic activity;
[0006] c), the direct smelting method requires a higher temperature, and requires a large amount of excess elemental phosphorus (because of the volatilization of the elemental phosphorus), and the crystal phase of the obtained product is mixed and difficult to control;
[0007] d) The TRP (temperature programmed reduction in hydrogen atmosphere) method is suitable for transition phosphate as a precursor, which has the advantages of low cost and high safety performance, and the obtained product is relatively pure, so it is the most widely used, but this method requires strict control of temperature rise Rate and reaction time, usually requires a long time to heat up (such as 2K / min or even 1K / min)

Method used

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  • Preparation method of transition metal phosphide with good morphology
  • Preparation method of transition metal phosphide with good morphology
  • Preparation method of transition metal phosphide with good morphology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 6.0g of cobalt chloride hexahydrate and 6.6g of sodium hypophosphite hydrate, and mix them evenly in a mortar; react the mixture at 800°C under the protection of argon for 60min; grind the obtained product into fine powder, wash with distilled water and absolute ethanol three times respectively , and then dried under vacuum at 60°C for 12 hours to obtain the product CoP.

[0035] figure 1 This is the XRD pattern of the obtained material. It can be seen from the comparison with the standard card that the synthesized material is a standard CoP.

[0036] figure 2 It is the TEM image of the prepared CoP. It can be seen from the figure that the CoP has a square regular structure.

[0037] image 3 It is the HR-TEM image of the prepared CoP. It can be seen from the figure that the lattice fringes of CoP are very obvious, and CoP is mainly stacked in face-centered cubic, and the exposed crystal plane is mainly (211) crystal plane, showing a single The crystal form, ...

Embodiment 2

[0039] Weigh 2.811g of cobalt sulfate heptahydrate and 1.255g of sodium hydrogen phosphite pentahydrate, and mix them uniformly in a mortar; react the mixture at 800°C under the protection of argon for 120min; grind the obtained product into fine powder, wash with distilled water and absolute ethanol three times respectively , and then vacuum dried at 80°C for 18h to obtain the product CoP.

[0040] Figure 4 This is the XRD pattern of the obtained material. It can be seen from the comparison with the standard card that the synthesized material is a standard CoP.

[0041] Figure 5 It is the TEM image of the prepared CoP. It can be seen from the figure that the CoP has a square regular structure.

[0042] Image 6 It is the HR-TEM image of the prepared CoP. It can be seen from the figure that the lattice fringes of CoP are very obvious, and CoP is mainly stacked in face-centered cubic, and the exposed crystal plane is mainly (211) crystal plane, showing a single The crysta...

Embodiment 3

[0044] Weigh 3.0g of nickel chloride hexahydrate and 6.6g of sodium hypophosphite hydrate, and mix them evenly in a mortar; react the mixture at 250°C under the protection of argon for 60min; grind the obtained product into fine powder, wash with distilled water and absolute ethanol three times respectively , and then vacuum dried at 60°C for 12h to obtain the product Ni 2 p.

[0045] Figure 7 It is the XRD pattern of the obtained material. It can be seen from the standard card that the synthesized material is the standard Ni 2 p.

[0046] Figure 8 For the prepared Ni 2 The TEM image of P, as can be seen from the figure, Ni 2 P is a rectangular regular structure.

[0047] Figure 9 For the prepared Ni 2 The HR-TEM image of P, as can be seen from the figure, Ni 2 The lattice fringes of P are very obvious, and Ni 2 P mainly stacks in the form of face-centered cubic, and the exposed crystal planes are mainly (111) crystal planes, and the crystal planes present a singl...

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Abstract

The invention relates to a preparation method of transition metal phosphide with good morphology, which is simple in process, and eliminates high temperature and high pressure complicated steps. The method comprises the following steps: taking a precursor of cobalt or nickel, and a precursor of phosphorus according to the molar ratio of (1:1)-(1:6); grinding and mixing the precursors uniformly; reacting for 60-240 minutes at 250-800 DEG C under the argon protection condition; porphyrizing the obtained product; using distilled water and absolute ethyl alcohol to respectively wash the product for three times; then drying the washed product at 60-80 DEG C for 12-24 hours, so as to obtain the product CoP or Ni2P. The main raw materials for the method are rich in sources and low in price, so that the cost is low; the synthetic method is novel, the process is simple, and the high temperature and high pressure complicated steps are not required, so as to simplify the preparation procedures and reduce the energy consumption; the prepared CoP and Ni2P are good in morphology, good in crystallization property, and have single crystal forms; the method disclosed by the invention cannot cause environment pollution during the preparation process, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of phosphide preparation, in particular to a method for preparing transition metal phosphide with good morphology. Background technique [0002] Transition metal phosphides are an important class of multifunctional materials, and their applications in catalysis and magnetism have attracted wide attention. Among them, CoP and Ni 2 P, as a low-cost, high-performance phosphide, has been widely studied and applied. [0003] Existing synthetic CoP and Ni 2 P's method has the following disadvantages: [0004] a), using organophosphorus or phosphine as a phosphorus source, which is highly toxic; [0005] b), hydrothermal synthesis cannot prepare supported phosphides, and the obtained product has poor catalytic activity; [0006] c), the direct smelting method requires a higher temperature, and requires a large amount of excess elemental phosphorus (because of the volatilization of the elemental phosphorus), and the crys...

Claims

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Application Information

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IPC IPC(8): C01B25/08
Inventor 邢巍常进法刘长鹏李晨阳梁亮张弘
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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