CN115321495A - Metal nitrogen-rich compound FeN 8 Method of synthesis of - Google Patents

Metal nitrogen-rich compound FeN 8 Method of synthesis of Download PDF

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Publication number
CN115321495A
CN115321495A CN202210894586.5A CN202210894586A CN115321495A CN 115321495 A CN115321495 A CN 115321495A CN 202210894586 A CN202210894586 A CN 202210894586A CN 115321495 A CN115321495 A CN 115321495A
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nitrogen
rich compound
mixture
fen
dac device
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CN115321495B (en
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吴刚
李贤丽
刘超
王升
王璐
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Northeast Petroleum University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/08—Hydrazoic acid; Azides; Halogen azides
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B35/00—Compositions containing a metal azide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention belongs to the technical field of synthesis of transition metal compounds, and particularly relates to a metal nitrogen-rich compound FeN 8 Mixing ferric chloride and sodium azide powder in a mass ratio of 4:5, and grinding the mixed material in a mortar until the particle size of material particles is less than 5 microns; 2. filling the ground mixture into a DAC device as a reaction precursor, and filling liquid argon into the DAC device to provide a hydrostatic pressure condition; 3. pressurizing the mixture to 50GPa through a DAC device; 4. heating the mixture by a laser heater, wherein the laser power is 20W, and the heating time is 12 minutes, and finally obtaining the metal nitrogen-rich compound FeN 8 . Process for the synthesis of nitrogen-enriched metal compounds, in which the nitrogen atom is represented by N, from metal chlorides and azides 6 The unit form exists, the energy density can reach 2.06kJ/g, and the material is a potential high-energy-content material.

Description

Metal nitrogen-rich compound FeN 8 Method for synthesizing (2)
Technical Field
The invention belongs to the technical field of synthesis of transition metal compounds, and particularly relates to a metal nitrogen-rich compound FeN 8 The method of (1).
Background
The nitrogen-rich compound is a high-energy density material with great potential, and the product after the nitrogen-rich compound releases energy is nitrogen gas which is environment-friendly. The basis for the high energy content of nitrogen-rich compounds is the difference in bond energy between the different nitrogen bonds, and a large amount of energy is released during the transition from single/double bonds to triple bonds. Therefore, the synthesis of the metal nitrogen-rich compound with low-bond nitrogen-nitrogen bonds provides a new idea for exploring and designing high-energy-density materials.
The existing synthesis of iron-nitrogen compounds adopts iron simple substance or iron nitride and liquid nitrogen as precursors, wherein the liquid nitrogen is used as a nitrogen source, and triple bonds in nitrogen molecules are opened under the conditions of high temperature and high pressure, so that Fe-N nitrogen-rich compounds are synthesized. The uniqueness of the precursor and nitrogen source limits the richness of the reaction product to some extent.
Disclosure of Invention
The invention overcomes the limitation of the singleness of the precursor and the nitrogen source in the background technology, provides a preparation method for synthesizing a novel metal nitrogen-rich compound by using metal chloride and azide under the conditions of high temperature and high pressure, and widens the exploration path for the research of the field of high-energy-content materials.
The technical scheme adopted by the invention is as follows: metal nitrogen-rich compound FeN 8 The metal nitrogen-rich compound FeN 8 The synthesis method comprises the following steps:
step one, ferric chloride and sodium azide (NaN) 3 ) Mixing the powder according to a mass ratio of 4:5, and grinding the mixed material in a mortar until the particle size of material particles is less than 5 microns;
step two, the mixture ground in the step one is loaded into a DAC device to serve as a reaction precursor, and liquid argon is filled into the DAC device to provide a hydrostatic pressure condition;
thirdly, pressurizing the mixture to 50GPa through a DAC device;
step four, heating the mixture by a laser heater, wherein the laser power is 20W, and the heating time is 10-15 minutes, and finally obtaining the metal nitrogen-rich compound FeN 8 。
Further, the heating time of the laser heater is 12 minutes.
The invention has the beneficial effects that: provides a preparation method for synthesizing a novel metal nitrogen-rich compound by using metal chloride and azide under the conditions of high temperature and high pressure, and widens the exploration path for the research of the field of high-energy-content materials. Compared with the existing Fe-N nitrogen-enriched compound synthesis technology, the method has the advantages that ferric chloride and sodium azide are used as precursors, the limitation of the existing precursors is broken through, wherein the sodium azide is used as a nitrogen source, a laser heating technology and a diamond anvil cell device (DAC device) are used for providing a high-temperature high-pressure environment, the precursors are subjected to displacement reaction, and a chemical formula of FeN is formed 8 The novel metal nitrogen-rich compounds of (1). The nitrogen atom in the compound is N 6 The unit form exists, the energy density can reach 2.06kJ/g, and the material is a potential high-energy-content material. And the liquid argon is used as a pressure transmission medium, so that the liquid argon is easier to encapsulate compared with liquid nitrogen, and the sample encapsulation cost is reduced.
Drawings
FIG. 1 is a layered FeN 8 A structural diagram of (1) (wherein a large sphere represents an Fe atom and a small sphere represents an N atom);
FIG. 2 is a graph showing a result of refinement of an XRD pattern.
Detailed Description
Example one
Metal nitrogen-rich compound FeN 8 The metal nitrogen-rich compound FeN 8 The synthesis method comprises the following steps:
step one, ferric chloride and sodium azide (NaN) 3 ) Mixing the powder according to a mass ratio of 4:5, and grinding the mixed material in a mortar until the particle size of material particles is less than 5 microns;
step two, the mixture ground in the step one is loaded into a DAC device to serve as a reaction precursor, and liquid argon is filled into the DAC device to provide a hydrostatic pressure condition;
thirdly, pressurizing the mixture to 50GPa through a DAC device;
and step four, heating the mixture by a laser heater, wherein the laser power is 20W, and the heating time is 12 minutes.
Example two
A DAC device with a diamond anvil surface of 300 mu m is selected, a rhenium sheet is used as a sealing pad material, the rhenium sheet is pre-pressed to 22GPa by the DAC device, and an indentation with the thickness of 40 mu m and the diameter of 300 mu m is obtained. A hole with the diameter of 150 μm is punched in the center of the indentation by a laser puncher and is used as a sample cavity for subsequent high-temperature high-pressure synthesis. The pressure in the sample cavity is calibrated by ruby, and three ruby balls with the diameter of 10-20 mu m are respectively placed on the upper anvil surface and the lower anvil surface of the DAC device. The iron chloride powder and sodium azide were then mixed in a mass ratio of 4:5 and ground in a mortar to a particle size of less than 5 μm, and a block of the mixture of iron chloride and sodium azide with a linearity of about 40 μm was selected. The selected mixture is placed in the sample cavity by using a tungsten filament, and the condition that the ruby ball on the DAC device can support the mixture block and the reaction precursor cannot directly contact with the anvil surface is ensured, so that the damage to the anvil surface of the diamond is reduced when the precursor is heated by laser. And then, closing the DAC device, placing the DAC device in liquid argon, screwing a pressurizing screw after the liquid argon flows into the sample cavity, pressurizing to 50GPa, and starting laser heating.
YLF laser is used as a heating light source, the laser is focused into a sample cavity through a heating light path, and the temperature in the sample cavity is controlled by adjusting the laser power. Slowly increasing the pressure from 0W to 20W, heating for 12min, and synthesizing the metal nitrogen-rich compound FeN 8 。（FeN 8 The crystal structure is shown in figure 1).
Metallic nitrogen-rich compound FeN 8 The method comprises the following steps of (1) performing synchrotron radiation X-ray diffraction data acquisition by using a Beijing synchrotron radiation device (BSRF) of China high-energy physics research institute, wherein the light source wavelength is 0.6199A, and the spectrum acquisition time is 60s. The directly obtained two-dimensional distribution of the spatial diffraction intensity is converted into an XRD diffraction spectrum of the diffraction intensity relative to the diffraction angle through FIT2D software integration. The XRD pattern was then subjected to crystal structure refinement analysis using Materials Studio 7.0 software. (the XRD pattern is shown in FIG. 2). The XRD pattern can be matched with metal nitrogen-enriched compound FeN 8 Precision matching (space group)P2 1 /c) Lattice parameters a =4.050 (5) a, b =8.005 (8) a, c =6.666 (2) a, β =72.688 (6) °.

Claims (2)

1. Metal nitrogen-rich compound FeN 8 The synthesis method is characterized in that: the metal nitrogen-rich compound FeN 8 The synthesis method comprises the following steps:
step one, mixing ferric chloride and sodium azide powder according to a mass ratio of 4:5, and grinding the mixed material in a mortar until the particle size of material particles is less than 5 microns;
step two, the mixture ground in the step one is loaded into a DAC device to serve as a reaction precursor, and liquid argon is filled into the DAC device to provide a hydrostatic pressure condition;
thirdly, pressurizing the mixture to 50GPa through a DAC device;
step four, heating the mixture by a laser heater, wherein the laser power is 20W, and the heating time is 10-15 minutes, and finally obtaining the metal nitrogen-rich compound FeN 8 。
2. The metal nitrogen-rich compound FeN according to claim 1 8 The synthesis method is characterized in that: the heating time of the laser heater is 12 minutes.
CN202210894586.5A 2022-07-28 2022-07-28 Metal nitrogen-rich compound FeN 8 Is synthesized by the method of (2) Active CN115321495B (en)

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