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Synthesis method of layered rhenium-nitrogen compound ReN2

A synthesis method and compound technology, which is applied in the field of transition metal compound synthesis, can solve the problems of cumbersome operation and increased investment in experimental resources, and achieve the effects of good synthesis safety, simple experimental preparation process, and high repeatability

Inactive Publication Date: 2016-07-13
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the reactants used are sensitive to the water and oxygen content of the environment, the preparation process of the experiment needs to be carried out in a glove box, and the operation is cumbersome.
If the synthesized ReN 2 To carry out further experimental research, a series of more complicated preparations are required to install it in the corresponding experimental device, which increases the resource input of the experiment.

Method used

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  • Synthesis method of layered rhenium-nitrogen compound ReN2
  • Synthesis method of layered rhenium-nitrogen compound ReN2
  • Synthesis method of layered rhenium-nitrogen compound ReN2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 layered ReN 2 Synthesis

[0020] Choose a DAC device with a diamond anvil surface of 300 μm (such as figure 1 ), using rhenium sheet as the gasket material, the rhenium sheet was pre-pressed to a thickness of 40 μm with a DAC device, and a hole with a diameter of 140 μm was punched in the center of the indentation with an electric spark puncher as a sample cavity. In order to reduce the damage caused by laser heating to the diamond anvil, four rubies with a particle size of 20-30 μm were placed on the upper and lower anvil surfaces of the DAC device as a heat insulation layer to avoid contact between the reactants and the diamond anvil surface. To calibrate the pressure in the sample chamber. Rhenium powder and NaN 3 Mix well in a mortar with a ratio of 1:2, pick a piece of Re, NaN after grinding 3 The mixture sample is put into the sample cavity, the sample diameter is 80 μm, and the thickness is 30 μm. The DAC device is closed and placed in liquid argon,...

Embodiment 2

[0023] Example 2 layered ReN 2 Characterization by X-ray Diffraction Pattern

[0024] Using the Advanced Photon Source APS (Advanced Photon Source) of the Argonne National Laboratory in the United States to collect synchrotron radiation X-ray diffraction data, the wavelength of the light source Spectrum acquisition time 5s. The directly obtained two-dimensional diffraction image was converted into a one-dimensional image of peak intensity versus diffraction angle by FIT2D software. Then use the Reflexmodule module in the MaterialsStudio7.0program to analyze the XRD image and match the peak position. (XRD pattern see image 3 )

[0025] The XRD pattern can be compared with the layered MoS reported in the previous literature 2 Type ReN 2 Matching (space group P63 / mmc), the lattice parameters obtained by structure refinement are XRD spectrum except ReN 2 There are also some miscellaneous peaks in the diffraction peaks. Through peak position identification, it can be det...

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Abstract

The invention provides a synthesis method of a layered rhenium-nitrogen compound ReN2 and belongs to the technical field of synthesis methods of transition metal compounds. The method comprises the following steps: mixing rhenium powder and sodium azide at a mass ratio of 1:2 so as to serve as raw materials, placing the mixture in a mortar, fully grinding, feeding the ground mixture into a DAC device, introducing liquid argon into the DAC device, then pressurizing the raw materials to 30 GPa, and performing laser heating for 8-12 minutes at a power of 20W, so as to obtain ReN2 with a layered structure. The raw materials used in the method are stable in air; the experimental preparation process is simple, the synthesis safety is good, and the repeatability is high.

Description

technical field [0001] The invention belongs to the technical field of synthesis methods of transition metal compounds, and relates to a new method for preparing layered ReN 2 s method. Background technique [0002] Compounds formed by light elements such as B, C, N, O and transition metals such as Re, Os, Yr have complex chemical bonds and generally have high hardness. But layered ReN 2 The hardness is unusually lower than other rhenium nitrogen compounds. The study of this anomalous phenomenon is beneficial to explore the physical mechanism of material changes under high temperature and pressure. [0003] Existing synthetic layered ReN 2 The technology can refer to Synthesis of rhenium nitride crystals with MoS2structure (Appl. Phys. Lett. 100, 2519102012). In this document, a large cavity press is used to make ReCl 5 with Li 3 N substitution reaction occurs under high temperature and high pressure. Since the reactants used are sensitive to the water and oxygen con...

Claims

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Application Information

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IPC IPC(8): C01B21/06
CPCC01B21/0615C01P2002/72
Inventor 崔田吴刚黄艳萍李芳菲黄晓丽
Owner JILIN UNIV
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