CN111233778A - High-temperature high-pressure preparation and normal-pressure capture method of limited-area high-density anhydrous alkali metal polymeric nitrogen NaN5 - Google Patents
High-temperature high-pressure preparation and normal-pressure capture method of limited-area high-density anhydrous alkali metal polymeric nitrogen NaN5 Download PDFInfo
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Abstract
The invention relates to the technical field of preparation of high-energy density materials, and provides a limited-range high-density anhydrous alkali metal polymeric nitrogen NaN5The high-temperature high-pressure preparation and normal-pressure capture method. The invention takes sodium azide of limited domain in a boron nitride nanotube as an initiator, and obtains limited domain high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure through high-pressure treatment5(ii) a After high pressure and laser heating treatment, the limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn2 which stably exists under high pressure is obtained1‑NaN5(ii) a After high pressure and laser heating treatment, the pressure is relieved, and the limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which stably exists under normal pressure is obtained5. The method is simple and easy to operate, and realizes the limited-area high-density anhydrous alkali metal polymeric nitrogen NaN for the first time5The preparation at high temperature and high pressure and the normal pressure capture provide an effective technical approach for the experimental preparation of the novel anhydrous alkali metal polymeric nitrogen.
Description
Technical Field
The invention relates to the technical field of preparation of high-energy density materials, in particular to a limited-range high-density anhydrous alkali metal polymeric nitrogen NaN5The high-temperature high-pressure preparation and normal-pressure capture method.
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, and since the N-N bond energy (160KJ/mol)/N ═ N bond energy (418KJ/mol) is much lower than the N ≡ N bond energy in nitrogen (954KJ/mol), it is depolymerized back to N upon its depolymerization2The molecules will release huge energy. The pentazole compound is a typical class of polymeric nitrogen materials, the nitrogen pentacyclic (N) of which5 -) The nitrogen atoms in (a) and (b) are on the same plane, and the nitrogen-nitrogen bond length is between that of a nitrogen-nitrogen single bond (N-N) and that of a nitrogen-nitrogen double bond (N ═ N).
In recent years, a plurality of pentazole salts which can stably exist under environmental conditions are obtained by chemical synthesis methods, wherein the pentazole salts comprise sodium-based pentazole salt [ Na ]8(N5)8(H2O)3]nAnd [ Na (N)5)(H2O)]·2H2And O. In the two sodium-based pentazole framework structures, sodium ions, bound water and free water stabilize nitrogen pentacyclic (N) in the sodium-based pentazole5 -) Plays an important role. It is worth noting that both the sodium-based pentazole framework structures contain a large amount of water molecules, the sodium-based pentazole structure cannot be separated from the water molecules and stably exists under the environmental condition, and the cage-shaped structures of the two sodium-based pentazole frameworks also cause the density of the sodium-based pentazole structure to be greatly reduced.
So far, the sodium-based pentazole structure only containing metal sodium ion coordination is not reported, and the anhydrous alkali metal polymeric nitrogen structure NaN with higher density5It has not been reported yet.
Disclosure of Invention
In view of the above, the present invention provides a limited-area high-density anhydrous alkali metal polymeric nitrogen NaN5The high-temperature high-pressure preparation and normal-pressure capture method. The invention obtains the stable-existing limited-range high-density anhydrous alkali metal polymeric nitrogen Cm-NaN under high pressure for the first time5And Pmn21-NaN5And realizes the capture of the stable existing limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN under normal pressure5。
In order to achieve the above object, the present invention provides the following technical solutions:
high density of a kind of limited areaAnhydrous alkali metal polymeric nitrogen Cm-NaN5The high pressure preparation method comprises the following steps:
sodium azide in a boron nitride nanotube in a confinement manner is packaged in a diamond anvil cell high-pressure cavity, and then the pressure is increased to more than 35GPa, so that the confined high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure is obtained5。
Limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5The high-temperature high-pressure preparation method comprises the following steps:
sodium azide in a boron nitride nanotube in a limited domain is packaged in a diamond anvil high-pressure cavity, the pressure is increased to more than 50GPa, then the laser heating treatment of 2000-2300K is carried out, and the limited-domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 stably existing under high pressure is obtained1-NaN5。
Confined high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN5The normal pressure interception method comprises the following steps:
encapsulating sodium azide limited in a boron nitride nanotube in a diamond anvil high-pressure cavity, pressurizing to more than 50GPa, then carrying out 2000-2300K laser heating treatment, and then relieving pressure to normal pressure to obtain limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN stably existing under normal pressure5。
Preferably, the pressurized pressure medium is liquid argon or liquid neon.
Preferably, the preparation method of the diamond anvil cell high-pressure cavity comprises the following steps: using a rhenium foil as a sealing pad material, and prepressing the rhenium foil by using a diamond anvil to form an indentation; and forming a hole in the center of the indentation by using a laser drilling machine to serve as a high-pressure cavity.
Preferably, the thickness of the rhenium foil after prepressing is 40-60 μm.
The invention provides the limited-range high-density anhydrous alkali metal polymeric nitrogen Cm-NaN obtained by the method in the scheme5。
The invention provides the limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn2 obtained by the method in the scheme1-NaN5。
The invention provides the limited-range high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN obtained by the method in the scheme5。
The invention provides a limited-range high-density anhydrous alkali metal polymeric nitrogen Cm-NaN5The high pressure preparation method comprises the following steps: sodium azide in a boron nitride nanotube in a confinement manner is packaged in a diamond anvil cell high-pressure cavity, and then the pressure is increased to more than 35GPa, so that the confined high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure is obtained5. The invention uses high pressure condition to make NaN3Structural phase transition occurs in which azide group N3 -Dissociate and polymerize to form N5 -Ring to obtain a stable existence of a limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN under high pressure5。
The invention provides a limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5The high-temperature high-pressure preparation method comprises the following steps: sodium azide in a boron nitride nanotube in a limited domain is packaged in a diamond anvil high-pressure cavity, the pressure is increased to more than 50GPa, then the laser heating treatment of 2000-2300K is carried out, and the limited-domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 stably existing under high pressure is obtained1-NaN5. The invention uses high temperature to promote NaN3Across the higher barrier to NaN5The structure is completely converted, and the crystallinity of the sodium nitrogen penta structure is better.
The invention also provides a limited-range high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN5The normal pressure interception method comprises the following steps: encapsulating sodium azide limited in boron nitride nanotubes in a diamond anvil high-pressure cavity, pressurizing to more than 50GPa, then carrying out 2000-2300K laser heating treatment, and then releasing pressure to obtain limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN stably existing at normal temperature and normal pressure5. The invention uses high temperature to promote NaN3To NaN5The structure is completely changed, the crystallinity of the sodium-nitrogen penta structure is better, and NaN is realized under the confinement effect of the boron nitride tube5And (4) normal pressure capture.
In addition, the high-temperature high-pressure preparation method and the normal-pressure capture method provided by the invention do not need harsh experimental conditions, and are simple and easy to operate.
Drawings
FIG. 1 shows Cm-NaN prepared in example 15The high-pressure in-situ Raman spectrum of @ BNNTs under the pressure of 35 GPa;
FIG. 2 is Cm-NaN prepared for example 15The high-pressure in-situ synchrotron radiation angle scattering XRD spectrogram of @ BNNTs under 35 GPa;
FIG. 3 shows Cm-NaN5、Pmn21-NaN5And P2/c-NaN5Wherein (a) is Cm-NaN5(ii) is a 3D crystal structure of (b) Pmn21-NaN5The 3D crystal structure of (c) is P2/c-NaN53D crystal structure diagram of (a);
FIG. 4 is Cm-NaN prepared in example 25The high-pressure in-situ Raman spectrum of @ BNNTs under the pressure of 43 GPa;
FIG. 5 is Cm-NaN prepared in example 25The high-pressure in-situ synchrotron radiation angle scattering XRD spectrogram of @ BNNTs under 43 GPa;
FIG. 6 is Cm-NaN prepared in example 35The high-pressure in-situ Raman spectrum of @ BNNTs under the pressure of 115 GPa;
FIG. 7 is Cm-NaN prepared in example 35High-pressure in-situ synchrotron radiation angle scattering (XRD) spectrogram of @ BNNTs under 115 GPa;
FIG. 8 is the Pmn2 prepared in example 41-NaN5The high-pressure in-situ Raman spectrogram of @ BNNTs under the pressure of 50 GPa;
FIG. 9 is the Pmn2 prepared in example 41-NaN5High-pressure in-situ synchrotron radiation angle scattering (XRD) spectrogram of @ BNNTs under 50 GPa;
FIG. 10 shows P2/c-NaN prepared in example 55Raman spectrogram under conditions of @ BNNTs, normal temperature and normal pressure;
FIG. 11 is P2/c-NaN prepared in example 55The synchrotron radiation XRD spectrogram of @ BNNTs under the conditions of normal temperature and normal pressure.
Detailed Description
The invention provides a limited-range high-density anhydrous alkali metal polymeric nitrogen Cm-NaN5The high-pressure preparation method of (1),the method comprises the following steps:
sodium azide in a boron nitride nanotube in a confinement manner is packaged in a diamond anvil cell high-pressure cavity, and then the pressure is increased to more than 35GPa, so that the confined high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure is obtained5。
In the invention, the preparation method of the diamond anvil cell high-pressure cavity is preferably as follows: the rhenium foil is used as a sealing pad material, the rhenium foil is pre-pressed by a diamond anvil, and a hole is formed in the center of the indentation by a laser drilling machine to be used as a high-pressure cavity. In the invention, the thickness of the rhenium foil after prepressing is preferably 40-60 μm; the diameter of the hole is preferably 1/3 of the anvil surface diameter of the diamond anvil, and in the specific embodiment of the invention, when the anvil surface diameter of the diamond anvil is 200 μm, the diameter of the hole is preferably 60-70 μm; the pressurized pressure transfer medium is preferably liquid argon or liquid neon, more preferably liquid argon, and in the embodiment of the invention, ruby microspheres with the diameter less than 10 μm are preferably used as the marking substance for calibrating the pressure in the high-pressure cavity.
In the invention, the sodium azide of the limited domain in the boron nitride nanotube is specifically NaN3The @ BNNTs confinement nano composite material is obtained by confining sodium azide in a boron nitride nanotube; the sodium azide with limited domain in the boron nitride nanotube has no special requirement, and can be prepared or purchased and used by using a method well known to the technical personnel in the field.
The invention encapsulates sodium azide confined in a boron nitride nanotube in a diamond anvil cell high-pressure cavity, then pressurizes the sodium azide to more than 35GPa, specifically 35GPa, 43GPa or 115GPa, and NaN is subjected to pressure action3Structural phase transition occurs in which azide group N3 -Dissociate and polymerize to form N5 -Ring formation to obtain NaN5The invention is prepared under high pressure, and particularly relates to high-density anhydrous alkali metal polymeric nitrogen NaN which stably exists under high pressure and is confined in a boron nitride nanotube5The space group is Cm, which is denoted as Cm-NaN5@ BNNTs (wherein BNNTs denotes boron nitride nanotubes).
The invention also provides a limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5The high-temperature high-pressure preparation method comprises the following steps:
sodium azide in a boron nitride nanotube in a limited domain is packaged in a diamond anvil high-pressure cavity, the pressure is increased to more than 50GPa, then the laser heating treatment is carried out at 2000-2300K, and the high-density anhydrous alkali metal polymeric nitrogen Pmn2 with the limited domain and the high density, which stably exists under high pressure, is obtained1-NaN5。
In the invention, the preparation method of the diamond anvil cell high-pressure cavity and the pressurized medium are the same as those in the scheme, and the details are not repeated herein; the sodium azide of the confinement in the boron nitride nanotube is consistent with the scheme, and is not described in detail herein.
After the packaging is finished, the invention is pressurized to more than 50GPa, specifically 50GPa or 60GPa, and then is subjected to 2000-2300K laser heating treatment, preferably 2100-2200K laser heating treatment. The invention preferably uses a fiber laser with the wavelength of 1064nm to carry out laser heating treatment, and the invention has no special requirements on the specific conditions of the laser heating treatment and can reach the required temperature. The invention utilizes laser to heat, and the high temperature can promote NaN3Across the higher barrier to NaN5The structure is completely changed, and the crystallinity of the sodium nitrogen penta structure is better; the invention is obtained by pressurizing and laser heating treatment, and particularly relates to high-density anhydrous alkali metal polymeric nitrogen NaN which stably exists under high pressure and is confined in a boron nitride nanotube5The space group is Pmn21Is recorded as Pmn21-NaN5@ BNNTs (wherein BNNTs denotes boron nitride nanotubes).
The invention also provides a limited-range high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN5The normal pressure interception method comprises the following steps:
encapsulating sodium azide in a boron nitride nanotube in a limited domain in a diamond anvil cell high-pressure cavity, pressurizing to more than 50GPa, then carrying out 2000-2300K laser heating treatment, and then relieving pressure to normal pressure to obtain the high-density non-localized sodium azide which stably exists under normal pressureAqueous alkali metal polymeric nitrogen P2/c-NaN5。
In the invention, the preparation method of the diamond anvil cell high-pressure cavity and the pressurized medium are the same as those in the scheme, and the details are not repeated herein; the sodium azide of the confinement in the boron nitride nanotube is consistent with the scheme, and is not described in detail herein.
After the packaging is finished, the invention is pressurized to more than 50GPa, specifically 50GPa, 53GPa or 58GPa, then is subjected to 2000-2300K laser heating treatment, preferably 2100-2200K laser heating treatment, and then is subjected to pressure relief. The invention preferably uses a fiber laser with the wavelength of 1064nm to carry out laser heating treatment, and the invention has no special requirements on the specific conditions of the laser heating treatment and can reach the required temperature. The invention utilizes laser to heat, and the high temperature can promote NaN3Across the higher barrier to NaN5The structure is completely changed, the crystallinity of the sodium-nitrogen penta structure is better, and NaN is realized under the confinement effect of the boron nitride tube5The normal pressure is intercepted; the invention is obtained under normal pressure, in particular to high-density anhydrous alkali metal polymeric nitrogen NaN which stably exists in a boron nitride nanotube under normal temperature and normal pressure and is confined in the boron nitride nanotube5The space group is P2/c and is marked as P2/c-NaN5@ BNNTs (wherein BNNTs denotes boron nitride nanotubes).
The invention also provides the limited-range high-density anhydrous alkali metal polymeric nitrogen Cm-NaN obtained by the method in the scheme5、Pmn21-NaN5And P2/c-NaN5. The invention obtains the anhydrous alkali metal polymeric nitrogen Cm-NaN with high density and limited range stably existing under high pressure for the first time5And Pmn21-NaN5(ii) a The invention utilizes the normal pressure interception method to obtain the limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN which stably exists under normal temperature and normal pressure for the first time5(ii) a Cm-NaN provided by the invention5、Pmn21-NaN5And P2/c-NaN5Is a sodium-based pentazole structure compound only coordinated by metal sodium ions, does not contain water molecules in the sodium-based pentazole skeleton structure, has higher energy density, and is based on NaN under corresponding pressure in the invention5The structure is decomposed intoNaN3And N2Calculation carried out at 35GPa Cm-NaN5Has a theoretical energy density of 103.2kJ/mol and Pmn2 at 50GPa1-NaN5The theoretical energy density of the catalyst is 114.7kJ/mol, and P2/c-NaN is at 0GPa5Has a theoretical energy density of 81.5 kJ/mol.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
Selecting a metal rhenium foil with anvil surface of 200 microns and purity of 99.97% as a sealing pad material, prepressing the sealing pad material by using the diamond anvil to form an impression, forming a circular hole with diameter of 70 microns at the center of the impression by using a laser drilling machine, and using the circular hole as a packaging NaN3A sample cavity of @ BNNTs confinement nanocomposite; liquid argon is filled in as a pressure transmission medium, and then ruby microspheres with the diameter less than 10 mu m are filled in as a marking substance for marking the pressure in the sample cavity. And rotating the diamond anvil pressing nut, and carrying out pressure loading under the normal temperature condition. When the pressure is raised to 35GPa, the limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN can be obtained5Is denoted as Cm-NaN5@BNNTs。
FIG. 1 and FIG. 2 are Cm-NaN, respectively5High-pressure in-situ Raman spectrogram of @ BNNTs under 35GPa (in the figure, the black arrow marks represent N5Characteristic vibration of the ring) and high pressure in situ synchrotron radiation angle dispersive XRD pattern (labeled Cm-NaN in the figure)5Phase diffraction peak), Cm-NaN in FIG. 3 (a)5The 3D crystal structure of (1). In the high-pressure in-situ Raman spectrum, the concentration is 400cm at 200--1The three characteristic peaks of (A) are NaN3High pressure phase gamma-NaN3(space group I4/mcm) at 650cm-1The characteristic peak is gamma-NaN3In N3 -At 1490cm of a bending vibration mode-1The characteristic peak of (A) is gamma-NaN3In N3 -Symmetric stretching vibration mode. The black arrows in the figure are marked with three new broad peaks, which is compared to Cm-NaN in theoretical prediction5The theoretical calculation of the structure shows that the Raman peak position is well matched, wherein the Raman peak position is positioned at 280cm-1Has a Raman vibration peak of N5 -Lattice vibration of the ring, at 800cm-1Has a Raman vibration peak of N5 -Ring bending vibration, located at 1100cm-1Has Raman vibration peak attribution of N5 -The ring is asymmetrically breathing and angularly deforming. In a high-pressure in-situ synchrotron radiation angle scattering XRD spectrogram, a new diffraction peak and Cm-NaN appear at 35GPa5The structure theory predicts that the map is well matched. In addition, at I4/mcm-NaN3Structure direction Cm-NaN5The process of structural phase change is accompanied by Cmmm-NaN2And (5) generating a structure.
Example 2
The press, sample chamber and pressure medium were the same as in example 1. Appropriate amount of domain-limited nano composite material NaN3@ BNNTs is filled into a sample cavity, ruby microspheres are added as a pressure mark (pressure in a detection pressure cavity), liquid argon is sealed as a pressure transmission medium, and pressurization is carried out. When the pressure is raised to 43GPa, the limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN can be obtained5@ BNNTs. FIGS. 4 and 5 are high-pressure in-situ Raman spectra of the sample at a pressure of 43GPa (the black arrows in the figures denote N)5 -The characteristic vibration of the ring. ) And high pressure in situ synchrotron radiation angular dispersive XRD (denoted as Cm-NaN in the figure)5Phase diffraction peaks), it can be seen from fig. 4 and 5 that NaN was successfully obtained under high pressure in this example5。
Example 3
The press, sample chamber and pressure medium were the same as in example 1. Appropriate amount of domain-limited nano composite material NaN3@ BNNTs is filled into a sample cavity, ruby microspheres are added as a pressure mark (pressure in a detection pressure cavity), liquid argon is sealed as a pressure transmission medium, and pressurization is carried out. When the pressure is raised to 115GPa, the polymer nitrogen NaN with limited area and high density and without water alkali metal can be obtained5Is denoted as Cm-NaN5@BNNTs。
The samples in the sample cavity were subjected to high pressure in situ Raman spectroscopy and high pressure in situ synchrotron radiation angular scattering, XRD, respectively, and the results were shown in fig. 6 and 7. Under the condition of 115GPa, the Raman spectrum shows NaN5Raman characteristic vibration of (1): wherein is located at 500cm of 300--1The Raman vibration peak of (A) is attributed to N5 -Lattice vibration of the ring, at 830cm-1The Raman vibration peak of (A) is attributed to N5 -Flexural vibration of the ring, located at 1160cm-1The Raman vibration peak of (A) is attributed to N5 -Asymmetric breathing and angular deformation vibration of the ring. Is positioned at 400-750cm-1In the range of N3 -Characteristic peak of bending vibration, and is located at 1560cm-1N of (A)3 -The symmetric stretching vibration characteristic peak disappears completely, and marks gamma-NaN3To NaN5Is completely converted. High-pressure in-situ synchrotron radiation XRD spectrogram and Cm-NaN5The results were consistent.
Example 4
The press, sample chamber and pressure medium were the same as in example 1. Appropriate amount of domain-limited nano composite material NaN3@ BNNTs is filled into a sample cavity, ruby microspheres are added as a pressure mark (pressure in a detection pressure cavity), liquid argon is sealed as a pressure transmission medium, and pressurization is carried out. When the pressure is raised to 50GPa, the sample in the sample cavity is subjected to high-pressure in-situ laser heating to 2000K to obtain the limited-area high-density anhydrous alkali metal polymeric nitrogen Pmn2 stably existing under high pressure1-NaN5@BNNTs。
FIG. 8 and FIG. 9 are respectively the Raman spectrum and the synchrotron radiation angle scattering XRD spectrum of the sample under the condition of 50GPa, and in FIG. 3, (b) is Pmn21-NaN5The 3D crystal structure of (1). Appearance of N in Raman spectrogram after laser heating5 -Characteristic vibration: wherein the center is located at 150-540cm-1Two Raman broadband of (2) belong to N5 -Lattice vibration of the ring, at 800cm-1The Raman vibration peak of (A) is attributed to N5 -Bending vibration of the ring at 1036, 1170cm-1The Raman vibration peak of (A) is attributed to N5 -Asymmetric breathing and angular deformation vibration of the ring. This is in accordance with the theoretical prediction of Pmn21-NaN5The theoretical calculation of the structure is good in Raman peak position matching. High-pressure in-situ synchrotron radiation angle scattering XRD spectrum and Pmn21-NaN5The results of the structure theory calculation maps are consistent.
Example 5
Press machineThe sample chamber and the pressure medium are the same as in example 1. Appropriate amount of domain-limited nano composite material NaN3@ BNNTs is filled into a sample cavity, ruby microspheres are added as a pressure mark (pressure in a detection pressure cavity), liquid argon is sealed as a pressure transmission medium, and pressurization is carried out. When the pressure is increased to 50GPa, the sample in the sample cavity is subjected to high-pressure in-situ laser heating to 2000K, then the sample is subjected to pressure relief to normal pressure, and the limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN existing under normal pressure is obtained5@BNNTs。
FIG. 10 and FIG. 11 are respectively the Raman spectrum and the synchrotron radiation angle scattering XRD spectrum of the sample under normal temperature and pressure conditions, and in FIG. 3, (c) is P2/c-NaN5The 3D crystal structure of (1). N appears in Raman spectrogram at normal temperature and normal pressure5 -Characteristic vibration peak at 119cm-1,831cm-1,998cm-1，1115cm-1And 1180cm-1This is in accordance with theoretical prediction of P2/c-NaN5The theoretical calculation of the structure is good in Raman peak position matching. Normal temperature and pressure synchrotron radiation angle scattering XRD spectrogram and P2/c-NaN5The results of the structure theory calculation maps are consistent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. Limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN5The high-pressure preparation method is characterized by comprising the following steps:
sodium azide in a boron nitride nanotube in a confinement manner is packaged in a diamond anvil cell high-pressure cavity, and then the pressure is increased to more than 35GPa, so that the confined high-density anhydrous alkali metal polymeric nitrogen Cm-NaN stably existing under high pressure is obtained5。
2. Limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5The high-temperature high-pressure preparation method is characterized by comprising the following steps of:
in goldSodium azide of a diamond anvil high-pressure cavity encapsulated in a limited domain in a boron nitride nanotube is pressurized to more than 50GPa, and then laser heating treatment is carried out at 2000-2300K to obtain limited domain high-density anhydrous alkali metal polymeric nitrogen Pmn2 stably existing under high pressure1-NaN5。
3. Confined high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN5The normal pressure interception method is characterized by comprising the following steps:
encapsulating sodium azide limited in a boron nitride nanotube in a diamond anvil high-pressure cavity, pressurizing to more than 50GPa, then carrying out 2000-2300K laser heating treatment, and then relieving pressure to normal pressure to obtain limited-area high-density anhydrous alkali metal polymeric nitrogen P2/c-NaN stably existing under normal pressure5。
4. The method of claim 1, 2 or 3, wherein the pressurized pressure transmitting medium is liquid argon or liquid neon.
5. The method of claim 1, 2 or 3, wherein the diamond anvil high pressure chamber is prepared by: using a rhenium foil as a sealing pad material, and prepressing the rhenium foil by using a diamond anvil to form an indentation; and forming a hole in the center of the indentation by using a laser drilling machine to serve as a high-pressure cavity.
6. The method as claimed in claim 5, wherein the thickness of the pre-pressed rhenium foil is 40 to 60 μm.
7. A limited-range high-density anhydrous alkali metal polymer nitrogen Cm-NaN obtained by the method of any one of claims 1 and 4 to 65。
8. The limited-range high-density anhydrous alkali metal polymeric nitrogen Pmn2 obtained by the method of any one of claims 2 and 4 to 61-NaN5。
9. The limited-area high-density anhydrous alkali metal polymer nitrogen P2/c-NaN obtained by the method of any one of claims 3 and 4-65。
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| CN111960391A (en) * | 2020-09-01 | 2020-11-20 | 吉林大学 | High-pressure preparation method of sodium pentazole |
| CN113717119A (en) * | 2021-03-19 | 2021-11-30 | 吉林大学 | Pentazole compound material and preparation method thereof |
| CN114408878A (en) * | 2022-01-11 | 2022-04-29 | 吉林大学 | High-temperature high-pressure preparation and low-temperature normal-pressure capture method of sodium pentazole |
| CN116002634A (en) * | 2022-12-29 | 2023-04-25 | 浙江大学杭州国际科创中心 | Cubic deflection structure polymeric nitrogen and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111847401A (en) * | 2020-07-27 | 2020-10-30 | 北华大学 | Preparation method of noble metal nitride nano material |
| CN111847401B (en) * | 2020-07-27 | 2022-12-27 | 北华大学 | Preparation method of noble metal nitride nano material |
| CN111960391A (en) * | 2020-09-01 | 2020-11-20 | 吉林大学 | High-pressure preparation method of sodium pentazole |
| CN113717119A (en) * | 2021-03-19 | 2021-11-30 | 吉林大学 | Pentazole compound material and preparation method thereof |
| CN114408878A (en) * | 2022-01-11 | 2022-04-29 | 吉林大学 | High-temperature high-pressure preparation and low-temperature normal-pressure capture method of sodium pentazole |
| CN114408878B (en) * | 2022-01-11 | 2023-03-21 | 吉林大学 | High-temperature high-pressure preparation and low-temperature normal-pressure capture method of sodium pentazole |
| CN116002634A (en) * | 2022-12-29 | 2023-04-25 | 浙江大学杭州国际科创中心 | Cubic deflection structure polymeric nitrogen and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
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| CN113387902B (en) | 2023-02-24 |
| CN111233778B (en) | 2021-09-14 |
| CN113387901B (en) | 2023-05-05 |
| CN113387902A (en) | 2021-09-14 |
| CN113387901A (en) | 2021-09-14 |
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