CN113387901B - Limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 High pressure process of (2) - Google Patents

Limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 High pressure process of (2) Download PDF

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CN113387901B
CN113387901B CN202110831146.0A CN202110831146A CN113387901B CN 113387901 B CN113387901 B CN 113387901B CN 202110831146 A CN202110831146 A CN 202110831146A CN 113387901 B CN113387901 B CN 113387901B
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CN113387901A (en
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刘冰冰
郭琳琳
刘波
刘然
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Jilin University
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Abstract

The invention relates to the technical field of high-energy density material preparation, and provides a limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Is a high-pressure process of (2). The invention uses the sodium azide in the boron nitride nano tube in a limited domainTo obtain limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN which is stable under high pressure by high-pressure treatment as a starting material 5 . The method provided by the invention has simple steps and easy operation, and realizes the limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN for the first time 5 Provides an effective technical approach for the experimental preparation of novel anhydrous alkali metal polymeric nitrogen.

Description

Limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 High pressure process of (2)
The application is that the application is carried out on the date of application of 2020, 1 month and 17 days, the application number of application is 202010053376.4, and the invention is a limited-domain high-density anhydrous alkali metal polymeric nitrogen NaN 5 The application of the high-temperature high-pressure preparation and normal-pressure interception method is applied to Jilin university.
Technical Field
The invention relates to the technical field of high-energy density material preparation, in particular to a finite-field high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Is a high-pressure process of (2).
Background
Polymeric nitrogen is a typical High Energy Density Material (HEDM) in which the nitrogen atoms are linked by N-N bonds or N=N bonds, which depolymerize to N due to the N-N bond energy (160 KJ/mol)/N=N bond energy (418 KJ/mol) being much lower than the N≡N bond energy (954 KJ/mol) in nitrogen 2 The molecules will release a great deal of energy. The tetrazole compounds are a typical class of polymeric nitrogen materials, whose azapentacyclic (N 5 - ) The nitrogen atoms in (a) are on the same plane, and the bond length of the nitrogen-nitrogen bond is between the single bond of nitrogen and nitrogen (N-N) and the double bond (N=N).
In recent years, a number of stable salts of tetrazoles including sodium-based salts of tetrazoles [ Na ] have been obtained by chemical synthesis 8 (N 5 ) 8 (H 2 O) 3 ] n [ Na (N) 5 )(H 2 O)]·2H 2 O. In these two sodium groups fiveIn the azole skeleton structure, sodium ions, bound water and free water pair stabilize the nitrogen pentacyclic (N) 5 - ) Plays an important role. It is notable that a large amount of water molecules are contained in both sodium-based tetrazole skeleton structures, wherein the sodium-based tetrazole structures cannot be separated from the water molecules to exist stably under the environmental conditions, and the cage-like structures of the two sodium-based tetrazole skeletons also result in a great reduction in the density of the sodium-based tetrazole structures.
To date, sodium-based tetrazole structures containing only metal sodium ion coordination have not been reported, and anhydrous alkali metal polymeric nitrogen structures NaN with higher densities have been reported 5 There is no report yet.
Disclosure of Invention
In view of this, the present invention provides a confined high density anhydrous alkali metal polymeric nitrogen NaN 5 High-temperature high-pressure preparation and normal-pressure interception methods. The invention obtains the limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN which can exist stably under high pressure for the first time 5 Pmn2 1 -NaN 5 And realize interception and stable existence of the confined high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN under normal pressure 5
In order to achieve the above object, the present invention provides the following technical solutions:
limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Comprises the following steps:
packaging sodium azide with a confinement in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, and then pressurizing to above 35GPa to obtain a confinement high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure 5
Limited high-density anhydrous alkali metal polymeric nitrogen Pmn2 1 -NaN 5 The high-temperature and high-pressure preparation method comprises the following steps:
packaging sodium azide with a limiting domain in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, and then performing 2000-2300K laser heating treatment to obtain the limiting domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 which stably exists under high pressure 1 -NaN 5
Limited high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN 5 The normal pressure interception method comprises the following steps:
packaging sodium azide with a limiting domain in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, then performing 2000-2300K laser heating treatment, and then releasing pressure to normal pressure to obtain the limiting domain high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which exists stably under the normal pressure 5
Preferably, the pressurized pressure transmission medium is liquid argon or liquid neon.
Preferably, the preparation method of the diamond anvil cell high-pressure cavity comprises the following steps: using rhenium foil as a sealing gasket material, and prepressing the rhenium foil by utilizing a diamond anvil cell to form an indentation; and forming a hole in the center of the indentation by using a laser puncher to serve as a high-pressure cavity.
Preferably, the thickness of the pre-pressed rhenium foil is 40-60 μm.
The invention provides the finite field high-density anhydrous alkali metal polymeric nitrogen Cm-NaN obtained by the method 5
The invention provides the finite field high-density anhydrous alkali metal polymeric nitrogen Pmn2 obtained by the method 1 -NaN 5
The invention provides the finite field high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN obtained by the method 5
The invention provides a limited-domain high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Comprises the following steps: packaging sodium azide with a confinement in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, and then pressurizing to above 35GPa to obtain a confinement high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure 5 . The invention utilizes high pressure condition to make NaN 3 Structural phase change occurs in which azide N 3 - Dissociating and polymerizing to form N 5 - A ring, thereby obtaining a confined high density anhydrous alkali metal polymeric nitrogen Cm-NaN which can exist stably under high pressure 5
The invention is thatProvides a confined high-density anhydrous alkali metal polymeric nitrogen Pmn2 1 -NaN 5 The high-temperature and high-pressure preparation method comprises the following steps: packaging sodium azide with a limiting domain in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, and then performing 2000-2300K laser heating treatment to obtain the limiting domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 which stably exists under high pressure 1 -NaN 5 . The invention utilizes high temperature to promote NaN 3 Cross a higher barrier to NaN 5 The structure is completely converted, and the crystallinity of the Na-N pentastructure is better.
The invention also provides a finite field high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN 5 The normal pressure interception method comprises the following steps: packaging sodium azide with a limiting region in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, then performing 2000-2300K laser heating treatment, and then releasing pressure to obtain the limiting region high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which stably exists at normal temperature and normal pressure 5 . The invention utilizes high temperature to promote NaN 3 To NaN 5 The complete transformation of the structure and better crystallinity of the Na-N pentastructure are realized, and NaN is realized under the limited domain effect of the boron nitride tube 5 Is intercepted under normal pressure.
In addition, the high-temperature high-pressure preparation method and the normal-pressure interception method provided by the invention do not need harsh experimental conditions, and are simple and easy to operate.
Drawings
FIG. 1 is a Cm-NaN prepared in example 1 5 High-pressure in-situ Raman spectrum of@BNTs under 35GPa pressure;
FIG. 2 is a graph showing the Cm-NaN prepared in example 1 5 High-pressure in-situ synchronous radiation angular dispersion XRD spectrum of@BNTs under 35 GPa;
FIG. 3 is Cm-NaN 5 、Pmn2 1 -NaN 5 And P2/c-NaN 5 Wherein (a) is Cm-NaN 5 (b) is Pmn2 1 -NaN 5 (c) is P2/c-NaN 5 A 3D crystal structure diagram of (2);
FIG. 4 is a Cm-NaN prepared in example 2 5 High-pressure in-situ Raman spectrum of@BNTs under 43GPa pressure;
FIG. 5 is a Cm-NaN prepared in example 2 5 High-pressure in-situ synchronous radiation angular dispersion XRD spectrum of @ BNTs under 43 GPa;
FIG. 6 is a Cm-NaN prepared in example 3 5 High-pressure in-situ Raman spectrum of@BNTs under 115GPa pressure;
FIG. 7 is a Cm-NaN prepared in example 3 5 High-pressure in-situ synchronous radiation angular dispersion XRD spectrum of @ BNTs under 115 GPa;
FIG. 8 shows Pmn2 prepared in example 4 1 -NaN 5 High-pressure in-situ Raman spectrum of@BNTs under 50GPa pressure;
FIG. 9 shows Pmn2 prepared in example 4 1 -NaN 5 High-pressure in-situ synchronous radiation angular dispersion XRD spectrum of @ BNTs under 50 GPa;
FIG. 10 is a P2/c-NaN prepared in example 5 5 Raman spectrum at normal temperature and normal pressure;
FIG. 11 is a P2/c-NaN prepared in example 5 5 Synchronous radiation XRD spectrum of @ BNTs under normal temperature and pressure conditions.
Detailed Description
The invention provides a limited-domain high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Comprises the following steps:
packaging sodium azide with a confinement in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, and then pressurizing to above 35GPa to obtain a confinement high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure 5
In the invention, the preparation method of the diamond anvil cell is preferably as follows: the rhenium foil is used as a sealing gasket material, the rhenium foil is pre-pressed by a diamond anvil, and a hole is formed in the center of an indentation by a laser puncher to be used as a high-pressure cavity. In the present invention, the thickness of the pre-pressed rhenium foil is preferably 40 to 60 μm; the diameter of the hole is preferably 1/3 of the diameter of the anvil surface of the diamond anvil, and in the specific embodiment of the invention, when the diameter of the anvil surface of the diamond anvil is 200 mu m, the diameter of the hole is preferably 60-70 mu m; the pressurized pressure transmission medium is preferably liquid argon or liquid neon, more preferably liquid argon, and in a specific embodiment of the present invention, ruby microspheres of less than 10 μm are preferably used as a pressure marking substance for marking the pressure in the high pressure chamber.
In the invention, the sodium azide limited in the boron nitride nanotube is specifically NaN 3 the@BNTs confinement nanocomposite is obtained by confining sodium azide in a boron nitride nanotube; the invention has no special requirement on the sodium azide of the confinement in the boron nitride nanotube, and the sodium azide can be prepared or purchased by using a method well known to a person skilled in the art.
The method comprises the steps of packaging sodium azide with a limiting region in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, and then pressurizing to more than 35GPa, specifically 35GPa, 43GPa or 115GPa, under the action of pressure, naN 3 Structural phase change occurs in which azide N 3 - Dissociating and polymerizing to form N 5 - A ring, thereby obtaining NaN 5 The invention is prepared under high pressure, in particular to a high-density anhydrous alkali metal polymeric nitrogen NaN which exists stably under high pressure and is limited in a boron nitride nano tube 5 The space group is Cm, which is denoted as Cm-NaN 5 @BNTs (wherein BNTs represents boron nitride nanotubes).
The invention also provides a finite field high-density anhydrous alkali metal polymeric nitrogen Pmn2 1 -NaN 5 The high-temperature and high-pressure preparation method comprises the following steps:
packaging sodium azide with a limiting domain in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, and then performing 2000-2300K laser heating treatment to obtain the limiting domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 which stably exists under high pressure 1 -NaN 5
In the invention, the preparation method of the diamond anvil cell and the pressurizing medium are consistent with the above scheme, and are not repeated here; the sodium azide of the confinement region in the boron nitride nanotube is consistent with the above scheme, and will not be described herein.
After the encapsulation is completed, the invention is pressurized toThe pressure of 50GPa or more, specifically 50GPa or 60GPa, and then 2000 to 2300K laser heat treatment, preferably 2100 to 2200K laser heat treatment. The invention preferably uses a fiber laser with the wavelength of 1064nm for laser heating treatment, and the invention has no special requirement on specific conditions of the laser heating treatment and can reach the required temperature. The invention uses laser to heat, and the high temperature can promote NaN 3 Cross a higher barrier to NaN 5 The complete transformation of the structure and better crystallinity of the Na-N pentastructure are achieved; the invention is obtained by pressurizing and laser heating treatment, in particular to a high-density anhydrous alkali metal polymeric nitrogen NaN which exists stably under high pressure and is limited in boron nitride nano-tube 5 The space group is Pmn2 1 Is denoted as Pmn2 1 -NaN 5 @BNTs (wherein BNTs represents boron nitride nanotubes).
The invention also provides a finite field high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN 5 The normal pressure interception method comprises the following steps:
packaging sodium azide with a limiting domain in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, then performing 2000-2300K laser heating treatment, and then releasing pressure to normal pressure to obtain the limiting domain high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which exists stably under the normal pressure 5
In the invention, the preparation method of the diamond anvil cell and the pressurizing medium are consistent with the above scheme, and are not repeated here; the sodium azide of the confinement region in the boron nitride nanotube is consistent with the above scheme, and will not be described herein.
After the encapsulation is completed, the invention is pressurized to more than 50GPa, specifically 50GPa, 53GPa or 58GPa, then 2000-2300K laser heating treatment is carried out, preferably 2100-2200K laser heating treatment is carried out, and then pressure relief is carried out. The invention preferably uses a fiber laser with the wavelength of 1064nm for laser heating treatment, and the invention has no special requirement on specific conditions of the laser heating treatment and can reach the required temperature. The invention uses laser to heat, and the high temperature can promote NaN 3 Crossing overHigher barrier NaN 5 The complete transformation of the structure and better crystallinity of the Na-N pentastructure are realized, and NaN is realized under the limited domain effect of the boron nitride tube 5 Is intercepted under normal pressure; the invention is a high density anhydrous alkali metal polymeric nitrogen NaN in the limited domain in the boron nitride nanometer tube which is stable under normal temperature and normal pressure 5 The space group is P2/c, which is named as P2/c-NaN 5 @BNTs (wherein BNTs represents boron nitride nanotubes).
The invention also provides the finite field high-density anhydrous alkali metal polymeric nitrogen Cm-NaN obtained by the method 5 、Pmn2 1 -NaN 5 And P2/c-NaN 5 . The invention obtains the stable limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN under high pressure for the first time 5 Pmn2 1 -NaN 5 The method comprises the steps of carrying out a first treatment on the surface of the The invention utilizes the normal pressure interception method to obtain the confined high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which is stably existing at normal temperature and normal pressure for the first time 5 The method comprises the steps of carrying out a first treatment on the surface of the The Cm-NaN provided by the invention 5 、Pmn2 1 -NaN 5 And P2/c-NaN 5 The sodium-based pentazole compound coordinated by metal sodium ions only does not contain water molecules in the skeleton structure of the sodium-based pentazole compound, has higher energy density, and is based on NaN under corresponding pressure 5 Structural decomposition into NaN 3 And N 2 Calculation was performed, cm-NaN at 35GPa 5 Has a theoretical energy density of 103.2kJ/mol and Pmn2 at 50GPa 1 -NaN 5 Has a theoretical energy density of 114.7kJ/mol and P2/c-NaN at 0GPa 5 Has a theoretical energy density of 81.5kJ/mol.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention.
Example 1
Selecting diamond with 200 micrometers anvil surface to generate high pressure, using metal rhenium foil with 99.97% purity as sealing gasket material, pre-pressing the diamond anvil on the sealing gasket material to form an indentation, and forming a circular hole with 70 micrometers diameter in the center of the indentation by using a laser puncher to obtain the packaging NaN 3 Sample of @ BNTs limited-domain nanocompositeA product cavity; the pressure in the sample cavity is calibrated by filling liquid argon as a pressure transmission medium and then filling ruby microspheres with the diameter of less than 10 mu m as a pressure marking substance. And (3) rotating the diamond anvil pressing nut, and carrying out pressure loading under the normal temperature condition. When the pressure is increased to 35GPa, the limited-domain high-density anhydrous alkali metal polymeric nitrogen Cm-NaN can be obtained 5 Denoted as Cm-NaN 5 @BNNTs。
FIGS. 1 and 2 are Cm-NaN, respectively 5 High-pressure in-situ Raman spectrum of @ BNTs under 35GPa pressure (black arrow mark in the figure represents N) 5 - Characteristic vibration of the ring) and high-voltage in-situ synchrotron radiation angular dispersive XRD patterns (labeled Cm-NaN in the figure) 5 Phase diffraction peak), FIG. 3 (a) is Cm-NaN 5 3D crystal structure diagram of (c). In high pressure in situ Raman spectrum, at 200-400cm -1 Is NaN 3 High pressure phase gamma-NaN 3 (space group is I4/mcm) lattice vibration mode, which is 650cm -1 The characteristic peak is gamma-NaN 3 Middle N 3 - Is located at 1490cm -1 Is characterized by gamma-NaN 3 Middle N 3 - Is a symmetrical telescopic vibration mode of the device. The black arrows in the figure are marked with three new broad peaks, which are comparable to Cm-NaN in theoretical predictions 5 The theoretical calculation of the structure shows that the Raman peak position is well matched, wherein the Raman peak position is positioned at 280cm -1 Has a Raman vibration peak of N 5 - Lattice vibration of ring at 800cm -1 Has a Raman vibration peak of N 5 - Ring bending vibration at 1100cm -1 The Raman vibration peak of (2) is N 5 - Ring asymmetric breathing and angular deformation vibrations. In the XRD spectrum of high-pressure in-situ synchronous radiation angular dispersion, a new diffraction peak and Cm-NaN appear at 35GPa 5 The structure theory prediction spectrum is well matched. In addition, in I4/mcm-NaN 3 Structural direction Cm-NaN 5 In the process of structural phase transition, cmm-NaN is accompanied 2 And (5) generating a structure.
Example 2
The press, sample chamber and pressure medium were the same as in example 1. Proper amount of NaN as limited nanometer composite material 3 Filling the @ BNTs into a sample cavity, and adding ruby microspheres as a pressing agentAnd (3) a target (detecting the pressure in the pressure cavity), and sealing liquid argon is used as a pressure transmission medium to pressurize. When the pressure is raised to 43GPa, the limited-domain high-density anhydrous alkali metal polymeric nitrogen Cm-NaN can be obtained 5 @BNTs. FIGS. 4 and 5 are respectively high pressure in situ Raman spectra of a sample under a pressure of 43GPa (black arrows in the figures indicate N 5 - The characteristic vibration of the ring. ) And high-voltage in-situ synchrotron radiation angular dispersion XRD spectra (labeled as Cm-NaN in the figure) 5 Phase diffraction peaks), according to FIGS. 4 and 5, the present example successfully obtained NaN at high pressure 5
Example 3
The press, sample chamber and pressure medium were the same as in example 1. Proper amount of NaN as limited nanometer composite material 3 Filling the @ BNTs into a sample cavity, adding ruby microspheres as a pressure mark (detecting the pressure in the pressure cavity), and sealing liquid argon as a pressure transmission medium for pressurization. When the pressure is increased to 115GPa, the limited-domain high-density anhydrous alkali metal polymeric nitrogen NaN can be obtained 5 Denoted as Cm-NaN 5 @BNNTs。
The samples in the sample cavity were subjected to high-pressure in-situ Raman spectral characterization and high-pressure in-situ synchrotron radiation angular dispersive XRD characterization, respectively, with the results shown in fig. 6 and 7. Raman spectra showed NaN at 115GPa 5 Raman characteristic vibrations of (c): wherein is located at 300-500cm -1 The Raman vibration peak of (2) is attributed to N 5 - Lattice vibration of the ring at 830cm -1 The Raman vibration peak of (2) is attributed to N 5 - Bending vibration of ring at 1160cm -1 The Raman vibration peak of (2) is attributed to N 5 - Asymmetric respiration and angular deformation vibration of the ring. Is positioned at 400-750cm -1 Within N 3 - Characteristic peak of flexural vibration, and at 1560cm -1 N of (2) 3 - The characteristic peak of symmetrical telescopic vibration completely disappears, marking gamma-NaN 3 To NaN 5 Is a complete transition of (c). High-voltage in-situ synchrotron radiation XRD spectrum and Cm-NaN 5 The results were consistent.
Example 4
The press, sample chamber and pressure medium were the same as in example 1. Proper amount of NaN as limited nanometer composite material 3 @ BNTs filled intoAnd adding ruby microspheres into the sample cavity as a pressure mark (detecting the pressure in the pressure cavity), and sealing liquid argon as a pressure transmission medium for pressurizing. When the pressure is increased to 50GPa, the sample in the sample cavity is heated to 2000K by high-pressure in-situ laser, so as to obtain the limited-area high-density anhydrous alkali metal polymeric nitrogen Pmn2 which exists stably under high pressure 1 -NaN 5 @BNNTs。
FIGS. 8 and 9 are respectively the Raman spectrum and the synchrotron radiation angular dispersion XRD spectrum of the sample under 50GPa, and (b) in FIG. 3 is Pmn2 1 -NaN 5 3D crystal structure diagram of (c). N appears in Raman spectrogram after laser heating 5 - Characteristic vibration: wherein is located at 150-540cm -1 Is assigned to N 5 - Lattice vibration of ring at 800cm -1 The Raman vibration peak of (2) is attributed to N 5 - Bending vibration of the ring at 1036, 1170cm -1 The Raman vibration peak of (2) is attributed to N 5 - Asymmetric respiration and angular deformation vibration of the ring. This is in comparison with Pmn2 in theory 1 -NaN 5 The structural theory calculates that the Raman peak position is well matched. High-voltage in-situ synchronous radiation angular dispersion XRD spectrum and Pmn2 1 -NaN 5 And the structure theory calculation map results are consistent.
Example 5
The press, sample chamber and pressure medium were the same as in example 1. Proper amount of NaN as limited nanometer composite material 3 Filling the @ BNTs into a sample cavity, adding ruby microspheres as a pressure mark (detecting the pressure in the pressure cavity), and sealing liquid argon as a pressure transmission medium for pressurization. When the pressure is increased to 50GPa, the sample in the sample cavity is heated to 2000K by high-pressure in-situ laser, and then the sample is depressurized to normal pressure, so that the confined high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN existing under the normal pressure is obtained 5 @BNNTs。
FIGS. 10 and 11 are respectively a Raman spectrum and a synchrotron radiation angular dispersion XRD spectrum of a sample at normal temperature and normal pressure, and (c) in FIG. 3 is P2/c-NaN 5 3D crystal structure diagram of (c). N appears in normal temperature and normal pressure Raman spectrogram 5 - Characteristic vibration peak at 119cm -1 ,831cm -1 ,998cm -1 ,1115cm -1 And 1180cm -1 This is in contrast to the theoretical prediction of P2/c-NaN 5 The structural theory calculates that the Raman peak position is well matched. XRD spectrum of synchronous radiation angular dispersion at normal temperature and normal pressure and P2/c-NaN 5 And the structure theory calculation map results are consistent.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (3)

1. Limited high-density anhydrous alkali metal polymeric nitrogen Cm-NaN 5 Is characterized by comprising the following steps:
packaging sodium azide with a confinement in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, and then pressurizing to above 35GPa to obtain a confinement high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure 5 The method comprises the steps of carrying out a first treatment on the surface of the The pressurized pressure transmission medium is liquid argon or liquid neon.
2. The method of claim 1, wherein the diamond anvil cell is prepared by: using rhenium foil as a sealing gasket material, and prepressing the rhenium foil by utilizing a diamond anvil cell to form an indentation; and forming a hole in the center of the indentation by using a laser puncher to serve as a high-pressure cavity.
3. The method of claim 2, wherein the pre-pressed rhenium foil has a thickness of 40-60 μm.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104447684A (en) * 2013-09-17 2015-03-25 上海创诺制药有限公司 Pomalidomide crystal form and preparation method thereof

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3483274A (en) * 1966-11-17 1969-12-09 Chevron Res Stereoregular coordination catalyst system having nitrogen-containing polymers
EP2135313B1 (en) * 2007-04-12 2011-09-14 3M Innovative Properties Company High performance, high durability non-precious metal fuel cell catalysts
CN105540558B (en) * 2016-01-26 2017-12-01 吉林大学 One kind polymerization nitrogen and preparation method thereof
CN106748602B (en) * 2017-01-24 2018-09-07 南京理工大学 Green gases propellant is hydrated pentazole metal salt and preparation method thereof
CN110467581A (en) * 2018-05-11 2019-11-19 南京理工大学 A kind of anhydrous nonmetallic pentazole ion salt and preparation method thereof
CN109573966B (en) * 2019-01-22 2020-09-11 吉林大学 NaN3@ BNNTs confinement nano composite material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104447684A (en) * 2013-09-17 2015-03-25 上海创诺制药有限公司 Pomalidomide crystal form and preparation method thereof

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