CN116002634A - Cubic deflection structure polymeric nitrogen and preparation method and application thereof - Google Patents
Cubic deflection structure polymeric nitrogen and preparation method and application thereof Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 285
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 142
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006902 nitrogenation reaction Methods 0.000 title description 2
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 80
- 239000010432 diamond Substances 0.000 claims abstract description 80
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000011521 glass Substances 0.000 claims abstract description 32
- 238000011049 filling Methods 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 15
- 238000007373 indentation Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 13
- 229910052702 rhenium Inorganic materials 0.000 claims description 8
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 16
- 238000001237 Raman spectrum Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 8
- 238000001069 Raman spectroscopy Methods 0.000 description 7
- 229910021389 graphene Inorganic materials 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 238000010892 electric spark Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 239000003380 propellant Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 229910017464 nitrogen compound Inorganic materials 0.000 description 2
- 150000002830 nitrogen compounds Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910021396 non-graphitizing carbon Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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Abstract
The invention relates to a cubic deflection structure polymeric nitrogen, a preparation method and application thereof. The preparation method of the cubic deflection structure polymeric nitrogen comprises the following steps: providing a diamond anvil cell; and filling glass carbon into the diamond anvil cell, cooling to below-148 ℃, continuously filling liquid nitrogen, pressurizing to above 100GPa, heating to above 2100K, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond. The cubic deflection structure polymeric nitrogen prepared by the preparation method can be stably stored at normal temperature and normal pressure, and the storage time is long.
Description
Technical Field
The invention relates to the technical field of energetic materials, in particular to a cubic deflection structure polymeric nitrogen and a preparation method and application thereof.
Background
The total nitrogen compound is a candidate with application prospect for High Energy Density Materials (HEDM) such as propellant, explosive and the like. In the case of the total nitrogen compounds, the polymeric nitrogen is in particularThe energy of the square deflection structure polymeric nitrogen (cg-N) is highest, and theoretical calculation shows that the cg-N density is 3.9g cm -3 The specific impact is 500s, and the detonation pressure is more than ten times of HMX (HMX). Currently cg-N is mainly prepared by pressurizing a anvil (DAC) with diamond to 140GPa and compressing nitrogen at a high temperature of 2000K. However, cg-N obtained by this preparation method cannot be stably stored at normal temperature and normal pressure.
Although a method for preparing polymeric nitrogen by using a carbon nanotube or graphene material appears in the market, the method can realize stable storage of the polymeric nitrogen at normal temperature and normal pressure, the preparation method is complex in operation, the prepared polymeric nitrogen sample is nano-scale, the yield is low, and the stable storage time at normal temperature and normal pressure is very short, namely the service life is basically in the order of 1 microsecond.
From this, it is clear that the polymeric nitrogen obtained by the conventional production method, especially cubic deflection structure polymeric nitrogen (cg-N), still has a problem that it is difficult to stably preserve at normal temperature and pressure.
Disclosure of Invention
In view of the above, it is necessary to provide a cubic nitrogen polymer having a deflection structure, which can be stably stored at normal temperature and pressure and has a long storage time, and a method for producing the same and use thereof.
A preparation method of polymerized nitrogen with a cubic deflection structure comprises the following steps:
providing a diamond anvil cell;
and filling glass carbon into the diamond anvil cell, cooling to below-148 ℃, continuously filling liquid nitrogen, pressurizing to above 100GPa, heating to above 2100K, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond.
In one embodiment, in the step of pressurizing, the pressure is applied to 100GPa to 120GPa.
In one embodiment, in the step of cooling, the temperature is reduced to-148 ℃ to-196 ℃.
In one embodiment, the glass carbon is filled with 60% -80% and the liquid nitrogen is filled with 20% -40%.
In one embodiment, in the heating step, the heating is to 2100K-2500K.
In one embodiment, the method for preparing the diamond anvil cell comprises the following steps:
preparing a diamond anvil cell;
prepressing the sealing pad by utilizing the diamond anvil cell to form an indentation;
and punching and forming a hole in the center of the indentation, wherein the hole is used as a diamond anvil cell.
In one embodiment, the diameter of the anvil face of the diamond anvil cell is selected from 70 μm to 90 μm;
and/or the diameter of the hole is selected from 30-50 μm.
In one embodiment, the thickness of the sealing pad is selected from 240-260 μm, and the thickness of the sealing pad after prepressing is selected from 10-30 μm;
and/or the material of the sealing pad is selected from rhenium or tungsten.
A cubic deflection structured polymeric nitrogen prepared according to the method of preparing a cubic deflection structured polymeric nitrogen as described above.
Use of a cubic deflection structured polymeric nitrogen as described above in an energetic material.
According to the invention, the glass carbon is filled in the diamond anvil cell and then is refilled with liquid nitrogen, and the filled liquid nitrogen enters the pores of the glass carbon and is mixed into the glass carbon, so that the liquid nitrogen and the glass carbon can simultaneously synthesize the cubic deflection structure polymeric nitrogen and the diamond under high temperature and high pressure in a high temperature and high pressure environment formed by pressurizing and heating treatment, and the cubic deflection structure polymeric nitrogen in a high pressure state is sealed in the glass carbon when the glass carbon is converted into the diamond, so that the cubic deflection structure polymeric nitrogen encapsulated in the diamond is obtained. Therefore, when the pressure is released to normal pressure and the temperature is reduced to normal temperature, the cubic deflection structure polymeric nitrogen encapsulated in the diamond prepared by the invention can be stably stored, and the storage time is long.
Drawings
FIG. 1 is a schematic diagram of a process for preparing cubic deflection structured polymeric nitrogen encapsulated in diamond according to the present invention;
FIG. 2 is a Raman spectrum of polymeric nitrogen encapsulated in a cubic deflection structure in diamond prepared in example 1 of the present invention at normal temperature and pressure;
FIG. 3 is a 3D crystal structure diagram of the cubic deflection structured polymeric nitrogen prepared in example 1 of the present invention;
FIG. 4 is a Raman spectrum of polymeric nitrogen prepared in comparative example 1 of the present invention;
FIG. 5 is a Raman spectrum of polymeric nitrogen prepared in comparative example 3 of the present invention;
FIG. 6 is a Raman spectrum of polymeric nitrogen prepared in comparative example 5 of the present invention;
FIG. 7 is a Raman spectrum of the cubic deflection structured polymeric nitrogen prepared in example 1 of the present invention after being placed at normal temperature and pressure for one week.
Detailed Description
The present invention will be described in more detail below in order to facilitate understanding of the present invention. It should be understood, however, that the invention may be embodied in many different forms and is not limited to the implementations or embodiments described herein. Rather, these embodiments or examples are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments or examples only and is not intended to be limiting of the invention. As used herein, the optional scope of the term "and/or" includes any one of the two or more related listed items, as well as any and all combinations of related listed items, including any two or more of the related listed items, or all combinations of related listed items.
Referring to fig. 1, fig. 1 is a schematic diagram of a preparation flow of cubic deflection structure polymeric nitrogen provided by the invention, wherein a represents glassy carbon, B represents liquid nitrogen, C represents diamond, and D represents polymeric nitrogen. As shown in fig. 1, the liquid nitrogen and the glassy carbon are decomposed and re-bonded under the condition of high temperature (2100K or more) and high pressure (100 GPa or more), so that the cubic deflection structure polymeric nitrogen and the diamond are obtained, and the cubic deflection structure polymeric nitrogen is encapsulated in the diamond in a high-pressure state.
Specifically, the preparation method of the cubic deflection structure polymeric nitrogen provided by the invention comprises the following steps:
s1, providing a diamond anvil cell;
and S2, filling glass carbon into the diamond anvil cell, cooling to below-148 ℃, continuously filling liquid nitrogen, pressurizing to above 100GPa, heating to above 2100K, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond.
Vitreous carbon is a non-graphitizing carbon that combines the properties of glass and ceramic, and is an amorphous, nearly 100% sp, as opposed to crystalline graphite 2 The hybridized carbon material is prepared by sintering polymeric organic precursor, such as phenolic resin, furfuryl alcohol resin and the like, at high temperature in inert gas atmosphere. The whole body is black, and the surface is smooth and similar to glass, so the glass is called glassy carbon. Vitreous carbons can be divided into two classes, type I and type II. The type I glassy carbon is formed by sintering a polymeric organic matter at a temperature lower than 2000 ℃, and the interior of the type I glassy carbon is mainly composed of crimped graphene fragments with unordered orientation; the type II glassy carbon is sintered at a higher temperature (2500 ℃), and is a disordered multi-layer graphene three-dimensional matrix formed by stacking nano-scale self-assembled fullerene-like sphere structures. It can be seen that compared with graphene materials, glassy carbon belongs to a disordered structure and has a three-dimensional pore structure.
According to the invention, the glass carbon is utilized to be of a three-dimensional pore structure, so that liquid nitrogen filled in the sample cavity can enter into pores of the glass carbon, namely, the liquid nitrogen is mixed in the glass carbon, and the glass carbon can be converted into diamond under high temperature and high pressure. Thus, the glass carbon and the liquid nitrogen filled in the sample cavity are simultaneously converted into corresponding diamond and cubic deflection structure polymeric nitrogen under the high-temperature and high-pressure environment formed by heating and pressurizing, and the cubic deflection structure polymeric nitrogen is sealed in a diamond micro-diamond cabin in a high-pressure state. Therefore, when the pressure is relieved to normal pressure and the temperature is reduced to normal temperature, the cubic deflection structure polymeric nitrogen encapsulated in the diamond can exist stably at normal temperature and normal pressure, and the existence time is long.
In conventional methods of preparing polymeric nitrogen, for example: in the method for preparing the polymeric nitrogen which can be stored at normal temperature and normal pressure by utilizing the carbon nano tube and the graphene material, raw materials are firstly dissolved, subjected to ultrasonic treatment and then transferred into the carbon nano tube or the graphene material, so that the preparation method is complex, the amount of nitrogen atoms transferred into the carbon nano tube or the graphene material is relatively small, the content of the nitrogen atoms is nano-scale, and the yield of the polymeric nitrogen is low and is basically about 1 percent; meanwhile, the preservation time is short.
According to the preparation method of the cubic deflection structure polymeric nitrogen, raw material transfer is not required to be considered, only liquid nitrogen is required to be directly filled in a sample cavity containing glass carbon, and the amount of the filled liquid nitrogen and the amount of the glass carbon are both in a micron level and far larger than a nanometer level, so that the yield of the cubic deflection structure polymeric nitrogen in the cubic deflection structure polymeric nitrogen encapsulated in diamond obtained at high temperature and high pressure is more than 30%. Therefore, the preparation method of the cubic deflection structure polymeric nitrogen is simple, easy to operate and high in synthesis rate.
In one embodiment, in consideration of the phase inversion effect of the glass carbon and the liquid nitrogen and the synthesis amount of the polymerized nitrogen of the cubic deflection structure, in the step S1, the preparation method of the diamond anvil cell comprises the following steps:
s11, preparing a diamond anvil cell;
s12, prepressing the sealing pad by utilizing the diamond anvil cell to form an indentation;
s13, punching and forming a hole in the center of the indentation, wherein the hole is used as a diamond anvil cell.
Preferably, in step S11, the diameter of the anvil surface of the diamond anvil cell is selected from 70 μm to 90 μm, and more preferably, the diameter of the anvil surface of the diamond anvil cell is selected from 80 μm. By the arrangement, the diamond anvil cell can be further ensured to generate high pressure of more than 100 GPa.
In one embodiment, in step S12, the thickness of the sealing pad is selected from 240 μm to 260 μm, and the thickness of the sealing pad after pre-pressing is selected from 10 μm to 30 μm. By the arrangement, the sealing gasket can be ensured to have enough hardness after compression, and subsequent use is facilitated.
Preferably, the material of the seal is selected from rhenium or tungsten. Further preferably, the gasket is selected from rhenium flakes having a thickness of 250 μm and a size of 2.5mm by 2.5 mm.
In one embodiment, in step S13, an electric spark punch is used to punch a hole in the center of the indentation as a diamond anvil cell, the hole having a diameter selected from 30 μm to 50 μm. By the arrangement, enough high pressure can be further ensured to be generated, the subsequent pressure for converting liquid nitrogen and glass carbon is facilitated, and meanwhile, the synthesis amount of polymerized nitrogen of the cubic deflection structure can be increased.
After the diamond anvil cell is formed, the diamond anvil cell is reset to the diamond anvil cell.
In the invention, a diamond anvil cell is filled with glass carbon and liquid nitrogen, and the synthetic rate and the packaging effect of the polymerized nitrogen of the cubic deflection structure are considered, in one embodiment, the filling rate of the glass carbon is selected from 60% -80%, and the filling rate of the liquid nitrogen is selected from 20% -40%.
In the preparation method of the invention, liquid nitrogen is used as a raw material and a pressure transmission medium, so that the pressure transmission medium is not required to be arranged during pressurization.
Considering that liquid nitrogen can be boiled at normal temperature, the liquid nitrogen is difficult to stably fill into a diamond anvil cell at normal temperature, so that the synthesis rate of the cubic deflection structure polymeric nitrogen is affected.
In one embodiment, in step S2, the temperature is reduced to-148 ℃ to-196 ℃, so that the stable filling of liquid nitrogen in the diamond anvil cell can be better ensured, and the liquid nitrogen can better enter into the pores of the glass carbon, thereby improving the synthesis rate of the cubic deflection structure polymeric nitrogen.
Considering that the glassy carbon and the liquid nitrogen both need to be subjected to structural phase transformation under high temperature and high pressure, and the control of temperature and pressure can influence the crystal structures obtained by the phase transformation of the glassy carbon and the liquid nitrogen, in order to enable the glassy carbon and the liquid nitrogen to be better simultaneously transformed into corresponding diamond and cubic deflection structure polymeric nitrogen, in the step S2, the pressure is preferably increased to 100GPa-120GPa, and the heating is carried out to 2100K-2500K.
In one embodiment, in step S2, a laser is used to heat the laser to above 2100K, the laser wavelength being selected from 1060nm-1070nm. Preferably, the laser is a carbon dioxide laser. The invention uses laser to heat, with high heating efficiency, high temperature can be reached quickly, the high temperature can promote the liquid nitrogen to pass through higher potential barrier to completely transform to the cubic deflection structure polymeric nitrogen of the cubic net structure, and the cubic deflection structure polymeric nitrogen has better crystallinity.
The invention obtains the high-density cubic deflection structure polymeric nitrogen encapsulated in diamond which can exist stably under normal temperature and normal pressure through pressurization and laser heating.
Meanwhile, the invention also provides the cubic deflection structure polymeric nitrogen prepared by the preparation method of the cubic deflection structure polymeric nitrogen. The cubic deflection structure polymeric nitrogen is a polymer formed by bonding nitrogen atoms through nitrogen-nitrogen single bonds, and the space group of the crystal structure of the cubic deflection structure polymeric nitrogen is I2 1 3, its energy density is as high as 10.33KJ/g.
In addition, the invention also provides application of the cubic deflection structure polymeric nitrogen in energetic materials.
In one embodiment, the energetic material may be a propellant, an explosive, a propellant charge, an initiating charge, a pyrotechnic charge, or the like.
The cubic deflection structured polymeric nitrogen and its preparation method and application will be further described by the following specific examples.
In the specific embodiment of the present invention, a HORIBA HR EVOLUTION raman spectrometer is used to detect the obtained cubic deflection structure polymeric nitrogen encapsulated in diamond and the polymeric nitrogen respectively, so as to obtain a corresponding raman spectrum, wherein the spectrum scanning range is as follows: 100cm -1 -1200cm -1 Or 100cm -1 -1400cm -1 Laser wavelength: 532nm, resolution: 1cm -1 。
Example 1
Pre-pressing a rhenium sheet with the thickness of 250 mu m and the size of 2.5mm multiplied by 2.5mm by utilizing a diamond with the anvil surface of 80 mu m to form an indentation, forming a hole with the diameter of 40 mu m at the center of the indentation by utilizing an electric spark puncher, wherein the hole is used as a sample cavity of the diamond anvil; and filling the glass carbon into a sample cavity, cooling to-150 ℃, continuously filling liquid nitrogen, filling the whole sample cavity, and calibrating the pressure in the sample cavity by taking a Raman peak of diamond as pressure, wherein the filling rate of the glass carbon is 60%, the filling rate of the liquid nitrogen is 40%, sealing a diamond anvil cell, carrying out pressure loading, pressurizing to 110GPa, heating to 2100K by laser, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond. The yield of cubic deflection structured polymeric nitrogen encapsulated in diamond obtained in this example was 36%.
Raman analysis was performed on the cubic-deflection-structure polymeric nitrogen encapsulated in diamond of this example, respectively, fig. 2 is a raman spectrum of the cubic-deflection-structure polymeric nitrogen encapsulated in diamond under normal temperature and pressure conditions, and fig. 3 is a 3D crystal structure diagram of the cubic-deflection-structure polymeric nitrogen prepared in example 1. From 950cm in the Raman spectrum shown in FIG. 2 -1 Characteristic peaks of the cubic deflection structure polymeric nitrogen appear, which are well matched with theoretical calculation Raman peak positions of the theoretical prediction neutral cubic deflection structure polymeric nitrogen structure.
Meanwhile, the cubic deflection structure polymeric nitrogen prepared in this example was analyzed, and fig. 3 is a 3D crystal structure diagram of the cubic deflection structure polymeric nitrogen prepared in example 1, and the lattice constant was 0.345nm.
It can be seen that this example successfully obtained cubic deflection structured polymeric nitrogen encapsulated in diamond at high pressure and high temperature.
Example 2
Pre-pressing a rhenium sheet with the thickness of 250 mu m and the size of 2.5mm multiplied by 2.5mm by utilizing a diamond with the anvil surface of 80 mu m to form an indentation, forming a hole with the diameter of 30 mu m at the center of the indentation by utilizing an electric spark puncher, wherein the hole is used as a sample cavity of the diamond anvil; and filling the glass carbon into a sample cavity, cooling to-180 ℃, continuously filling liquid nitrogen, filling the whole sample cavity, and calibrating the pressure in the sample cavity by taking a Raman peak of diamond as pressure, wherein the filling rate of the glass carbon is 70%, the filling rate of the liquid nitrogen is 30%, sealing a diamond anvil cell, carrying out pressure loading, pressurizing to 120GPa, heating to 2200K by laser, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond. The yield of polymerized nitrogen of the cubic deflection structure encapsulated in diamond was 42%.
Example 3
Pre-pressing a tungsten sheet with the thickness of 250 mu m and the size of 2.5mm multiplied by 2.5mm by utilizing a diamond anvil with the anvil surface of 80 mu m to form an indentation, forming a hole with the diameter of 40 mu m in the center of the indentation by utilizing an electric spark puncher, wherein the hole is used as a sample cavity of the diamond anvil; and filling the glass carbon into a sample cavity, cooling to-170 ℃, continuously filling liquid nitrogen, filling the whole sample cavity, and calibrating the pressure in the sample cavity by taking a Raman peak of diamond as pressure, wherein the filling rate of the glass carbon is 80%, the filling rate of the liquid nitrogen is 20%, sealing a diamond anvil cell, carrying out pressure loading, pressurizing to 100GPa, heating to 2300K by laser, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond. The yield of polymerized nitrogen of the cubic deflection structure encapsulated in diamond was 48%.
Example 4
The difference from example 1 is that in example 4, the filling ratio of the vitreous carbon is 50% and the filling ratio of the liquid nitrogen is 50%. The yield of cubic deflection structured polymeric nitrogen encapsulated in diamond obtained in this example was 30%.
Example 5
In comparison with example 1, only the difference was that in example 5, a rhenium piece having a thickness of 240 μm and a size of 2.5mm×2.5mm was pre-pressed with a diamond anvil having an anvil surface of 70 μm to form an indentation, the pre-pressed rhenium piece having a thickness of 20 μm, and then a hole having a diameter of 25 μm was formed in the center of the indentation by an electric discharge punch, the hole serving as a sample cavity of the diamond anvil. The yield of cubic deflection structured polymeric nitrogen encapsulated in diamond obtained in this example was 36%.
Comparative example 1
The only difference compared to example 1 is that in comparative example 1, the glassy carbon was filled into the sample cavity, cooled to-130 ℃, and the liquid nitrogen was continuously filled to fill the entire sample cavity.
The raman spectrum of the polymeric nitrogen prepared in this comparative example is shown in fig. 4, and the polymeric nitrogen crystal structure is not a cubic deflection structure polymeric nitrogen.
Comparative example 2
The only difference compared to example 1 is that in comparative example 2, the glassy carbon was filled into the sample cavity, cooled to 0 ℃, and the filling with liquid nitrogen was continued to fill the entire sample cavity.
Comparative example 3
The difference compared to example 1 is only that in comparative example 3, the pressurization was to 90GPa.
The raman spectrum of the polymeric nitrogen prepared in this comparative example is shown in fig. 5, and the polymeric nitrogen crystal structure is not a cubic deflection structure polymeric nitrogen.
Comparative example 4
The difference compared to example 2 is only that in comparative example 4, the pressure was increased to 95GPa.
Comparative example 5
The only difference compared to example 1 is that in comparative example 5, heating to 2000K was performed.
The raman spectrum of the polymeric nitrogen prepared in this comparative example is shown in fig. 6, and the polymeric nitrogen crystal structure is not a cubic deflection structure polymeric nitrogen.
To better illustrate that the cubic deflection polymeric nitrogen prepared by the preparation method of the present invention can be stably stored at normal temperature and pressure, and the storage time is long, the applicant performs raman analysis after the cubic deflection polymeric nitrogen prepared in example 1 is placed at normal temperature and pressure for one week, and the result is shown in fig. 7. As is clear from FIG. 7, the cubic deflection polymeric nitrogen prepared by the preparation method of the present invention can be stored stably at normal temperature and pressure, and the storage time is long.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the cubic deflection structure polymeric nitrogen is characterized by comprising the following steps of:
providing a diamond anvil cell;
and filling glass carbon into the diamond anvil cell, cooling to below-148 ℃, continuously filling liquid nitrogen, pressurizing to above 100GPa, heating to above 2100K, and finally decompressing to normal pressure and cooling to normal temperature to obtain the cubic deflection structure polymeric nitrogen encapsulated in the diamond.
2. The method of preparing cubic deflection structured polymeric nitrogen according to claim 1, wherein in the step of pressurizing, the pressure is increased to 100GPa to 120GPa.
3. The method of preparing cubic deflection structured polymeric nitrogen according to claim 1, wherein in the step of cooling, the temperature is reduced to-148 ℃ to-196 ℃.
4. The method for preparing the cubic deflection structured polymeric nitrogen according to claim 1, wherein the filling rate of the glassy carbon is selected from 60% -80%, and the filling rate of the liquid nitrogen is selected from 20% -40%.
5. The method of preparing cubic deflection structured polymeric nitrogen according to claim 1, wherein in the heating step, the heating is performed to 2100K to 2500K.
6. A method of preparing cubic deflection structured polymeric nitrogen according to any one of claims 1 to 5, wherein the method of preparing the diamond-anvil sample chamber comprises the steps of:
preparing a diamond anvil cell;
prepressing the sealing pad by utilizing the diamond anvil cell to form an indentation;
and punching and forming a hole in the center of the indentation, wherein the hole is used as a diamond anvil cell.
7. The method of preparing cubic deflection structured polymeric nitrogen according to claim 6, wherein the diameter of the anvil face of the diamond anvil cell is selected from 70 μm to 90 μm;
and/or the diameter of the hole is selected from 30-50 μm.
8. The method of preparing cubic deflection structured polymeric nitrogen according to claim 6, wherein the thickness of the mat is selected from 240 μm to 260 μm and the thickness of the pre-pressed mat is selected from 10 μm to 30 μm;
and/or the material of the sealing pad is selected from rhenium or tungsten.
9. A cubic deflection structured polymeric nitrogen prepared by the method of preparing a cubic deflection structured polymeric nitrogen according to any one of claims 1 to 8.
10. Use of the cubic deflection structured polymeric nitrogen of claim 9 in energetic materials.
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