CN115819165A - Copper azide composite initiating explosive block material and preparation method thereof - Google Patents
Copper azide composite initiating explosive block material and preparation method thereof Download PDFInfo
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- 230000000977 initiatory effect Effects 0.000 title claims abstract description 12
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- 239000013148 Cu-BTC MOF Substances 0.000 claims abstract description 34
- 239000013590 bulk material Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 8
- 235000010413 sodium alginate Nutrition 0.000 claims description 8
- 239000000661 sodium alginate Substances 0.000 claims description 8
- 229940005550 sodium alginate Drugs 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
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- 238000005474 detonation Methods 0.000 abstract description 12
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- 150000001540 azides Chemical class 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
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- 239000007787 solid Substances 0.000 abstract description 2
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- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 239000012621 metal-organic framework Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
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- 238000000634 powder X-ray diffraction Methods 0.000 description 2
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- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000011159 matrix material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
The invention belongs to the crossing field of nano materials and coordination chemistry, and discloses a high-safety firm copper azide composite initiating explosive block material and a preparation method thereof. The method obtains precursor material MOF-199 hybrid material by locking MOF-199 in tightly connected polymer network. And then carrying out heat treatment and gas-solid azide reaction to obtain the CA-C bulk material. The CA-C block material shows various mechanical stability (such as good impact resistance, vibration resistance and overload resistance) under simulated working conditions. Meanwhile, the content of CA in the CA-C block material reaches up to 70.3 percent, and the detonation power of the CA-C block material is ensured. Moreover, the CA-C bulk material is assembled in the micro detonator, and CL-20 (secondary explosive) can be effectively detonated under the irradiation of laser. The material as a safe micro-detonation material provides good prospect for the wide application of the material in aerospace systems.
Description
Technical Field
The invention belongs to the crossing field of nano materials and coordination chemistry, relates to a high-safety composite initiating explosive block material and a preparation method thereof, and particularly relates to a firm copper azide composite material.
Background
Advances in nanotechnology have led to the development of miniaturized Initiating Explosive Devices (IEDs), which can significantly reduceThe volume and weight of aerospace, weaponry, and civil explosion systems. The primary explosive, which is a core component of the IED, can quickly complete the process from detonation to explosion when encountering a small external stimulus. Copper azide (Cu (N) 3 ) 2 CA) has excellent detonation capability and low toxicity, and is a promising micro-initiation material. However, CA is easily limited in practical use due to its high electrostatic sensitivity. However, studies have shown that the synthesis of CA encapsulated in a porous carbon network using Metal Organic Frameworks (MOFs) as sacrificial templates is an effective method to enhance CA electrostatic safety. MOFs are a class of crystalline materials that include a uniform arrangement of metal-containing nodes separated by organic linkers. The preparation of CA composites with MOF is highly advantageous due to its specific surface area and tunable chemical composition. Although some preliminary studies have been successful, the CA composites obtained are usually collected in the form of powders or films, which makes them difficult to implement in practical applications.
As the CA-C powder or the film in the micro detonator often generates violent vibration in the charging or detonating process, the reliability is poor. In harsh working environments, loaded CA powders are often affected by particle-polymer-matrix interactions and are therefore easily dislodged from the equipment, resulting in the occurrence of accidental explosions. Although the CA films prepared have advantages over powders, the high flexibility still leads to unsatisfactory mechanical stability. Furthermore, CA membranes are hindered by low detonation power due to the limited thickness of the membrane. Thus, there is a need for an adaptive method of making robust copper azide composite materials for safe micro-detonator applications.
Disclosure of Invention
The invention aims to develop a copper azide composite initiating explosive block material with high safety and firmness; another object is to develop an adaptive method for preparing the composite material.
To achieve the object of the invention, the invention employs a hybrid method, which results in a precursor material MOF-199 hybrid material by locking the MOF-199 in a tightly linked polymer network. And then carrying out heat treatment and gas-solid azide reaction to obtain CA particles uniformly fixed in a cross-linked carbon network, wherein the material obtained by the method is a CA-C bulk material.
The preparation method comprises the following steps:
(1) Preparation method of precursor material MOF-199 hybrid material) was as follows:
dissolving MOF-199 and sodium alginate in distilled water, and stirring until the mixture is uniformly dispersed. Meanwhile, respectively dissolving polyacrylic acid and anhydrous calcium chloride in distilled water, and mixing the two solutions to obtain a curing solution. The sodium alginate dispersion of MOF-199 was dropped into the solidification solution. And after the MOF-199 hybrid material is shaped, washing with distilled water and drying.
(2) The preparation method of the CA-C bulk material comprises the following steps:
the resulting MOF-199 hybrid material was placed in a tube furnace, heat treated under nitrogen, and then placed over a flowing HN 3 Reacting in gas to prepare the CA-C bulk material.
In the MOF-199 hybrid Material, ca 2+ Alginate and polyacrylic acid (PAA) were introduced as binders to ensure stability of the overall network. Multiple hydrogen and coordination bonds allow the MOF-199 hybrid material to maintain good stability (shown in FIG. 1).
The MOF-199 hybrid material is prepared using a continuous flow device, such as by adjusting the syringe size, the size of the MOF-199 hybrid material can be easily adjusted within certain limits. In addition, different molds can be used to mold the MOF-199 hybrid material in the desired shape (shown in FIG. 2). The self-adaptive preparation method can be better applied to a micro-detonating device and an energy-gathering charge technology.
The synthesized CA-C bulk material was initially characterized as follows: the successful synthesis of CA was demonstrated by powder X-ray diffraction Pattern (PXRD). Fourier-infrared spectrum display: 2119 and 2080cm -1 Peaks at the frequencies of symmetric vibration of the azide, 1300 and 1256cm -1 Peaks at (D) belong to the asymmetric vibration frequency of azides, 686 and 570cm -1 The peak at (A) belongs to Cu-N 3 Symmetrical extension of the Cu-N bond in the system. The chemical states of Cu, C and N in the CA-C bulk material were studied using X-ray photoelectron spectroscopy (XPS). In high resolution Cu 2p spectra, two dominant speciesPeaks at 953.2 and 933.1eV, satellite peaks at 963.3 and 943.0eV, respectively, assigned to Cu (II) 2p 1/2 And Cu (II) 2p 3/2 . The +2 oxidation state indicates that metallic Cu is fully converted to CA. Two peaks of the high-resolution N1s spectrum are respectively positioned at 403.1 eV and 399.3eV and are respectively assigned to-N 3 And Cu — N, also confirmed CA formation (shown in fig. 3).
The morphology of the CA-C bulk material is characterized as follows: the CA nanoparticles were embedded in the porous carbon network as observed by Transmission Electron Microscopy (TEM). In the high-resolution TEM (HR-TEM) image, the lattice fringes with a plane spacing of 0.291 and 0.319nm correspond to the (101) and (230) crystal planes of CA, respectively. Finally, selected Area Electron Diffraction (SAED) also shows the CA facets. Furthermore, the energy dispersive spectrometer element map (EDS-mapping) shows a uniform distribution of C, cu and N elements, indicating a good dispersion of CA in the carbon network (shown in fig. 4).
The stability of the CA-C bulk material and the CA powder in the microchip was tested as follows: the abrasion resistance test was conducted by adhesion to an adhesive tape, and it was observed that the conventional CA powder was easily separated from the substrate after peeling, and the CA-C bulk material did not fall off. The anti-vibration and impact properties of the CA-C bulk material and CA powder in the microchip were investigated using a grinder. The actual situation is simulated by adopting different vibration frequencies of 10 Hz, 20 Hz, 30 Hz and 40Hz, and the observation shows that no particles fall off after the CA-C block material vibrates for 10min, and the CA powder is completely dispersed. To further demonstrate the mechanical stability of the CA-C bulk material, we dropped the microchip with the sample from different heights, and the high speed photographs before and after dropping showed that the CA-C bulk material did not fall off the microchip at a height of 60cm, whereas the CA powder fell off the outside of the microchip. Finally, the load bearing characteristics of the CA-C bulk material and CA powder under high overload conditions were simulated with a high speed centrifuge. The result shows that the overload resistance of the CA-C block material-based micro detonator is more than 10000g. The simulation experiment shows that the CA-C block material has the performances of wear resistance, vibration resistance, impact resistance, overload resistance and the like, so that accidental explosion caused by particle scattering in practical application can be effectively prevented, and the performance of the CA-C block-based IED (shown in figure 5) is ensured.
The laser detonation test of the CA-C bulk material was as follows: laser light was started on the CA-C block material and at 16.1ms there was a large bright flame accompanied by a violent explosion and sound, the corresponding input energy was calculated to be 8.05mJ. In addition, a continuous explosion device is designed, and CA-C bulk materials are filled into the explosion point of the rotatable explosion device. A series of explosion transients captured with a high speed camera is shown in figure 6. Under the laser irradiation, the four light spots are triggered one by one to generate bright flames. It is worth emphasizing that when one of the points is triggered by the laser to explode, the other explosion points do not explode or fail, and the result further proves the high reliability of the CA-C bulk material. Furthermore, the CA-C bulk material successfully detonates the secondary explosive CL-20 in a laser triggered detonation system, demonstrating its excellent detonation capabilities (shown in FIG. 6).
The invention has the innovation points that: the safe and firm copper azide composite initiation explosive block material is prepared by a simple hybridization method by utilizing a mixed template of a metal-organic framework and a cross-linked polymer.
The invention has the advantages that: 1. the prepared CA-C block composite material has a required physical structure, and has the performances of wear resistance, vibration resistance, impact resistance, overload resistance and the like and excellent detonation capability. 2. This method locks the MOF-199 in a tightly linked polymer network, resulting in CA particles that are uniformly immobilized in a cross-linked carbon network. The CA-C bulk material prepared by the in-situ method inherits the hardness of the MOF and the softness of the polymer. Thus, the CA-C bulk material is made to exhibit significant mechanical stability (e.g., good impact and overload resistance) and desirable conformability when integrated into a micro-detonator (shown in fig. 7). Under 1064nm laser irradiation, the CA-C bulk material can be detonated one by one and continuously in a continuous explosion device, which further proves the reliability of the CA-C bulk material. Furthermore, the CA-C bulk material successfully detonated the secondary explosive CL-20 in a laser triggered micro-detonator. The material as a safe micro-detonation material provides good prospect for the wide application of the material in aerospace systems.
Drawings
FIG. 1 is a graph of multiple cross-linking events in a MOF-199 hybrid material according to the invention.
FIG. 2 is a graph of MOF-199 hybrid materials and CA-C bulk materials of different sizes and shapes according to the present invention.
FIG. 3 is a preliminary characterization test pattern of the CA-C bulk material of the present invention.
FIG. 4 is a pattern of the CA-C bulk material of the present invention.
FIG. 5 is a graph of the stability test of the CA-C bulk material and CA powder of the present invention in a microchip.
FIG. 6 is a laser detonation test pattern of the CA-C bulk material of the present invention.
FIG. 7 is a schematic diagram of the preparation route and application of the present invention.
Detailed Description
The invention is further illustrated by the following examples:
example 1: synthesis of the MOF-199 hybrid materials of the invention.
7.5g of MOF-199 and 3.5g of sodium alginate were dissolved in 50mL of distilled water and stirred until uniformly dispersed. Meanwhile, 0.204g of polyacrylic acid (PAA) and 250mg of anhydrous calcium chloride were dissolved in 10mL of distilled water, respectively, and the two solutions were mixed to prepare a solidified solution. Then, the sodium alginate dispersion of MOF-199 was dropped into the solidification solution. And after the MOF-199 hybrid material is shaped, washing with distilled water for many times, and drying at 60 ℃.
Example 2: synthesizing the CA-C bulk material.
And (3) placing the obtained MOF-199 hybrid material in a tube furnace for heat treatment, heating to 500 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, keeping for 30min, and naturally cooling to room temperature. A round bottom flask was charged with 0.5g NaN 3 And 2.75g stearic acid, heated to 125 ℃ to give HN 3 A gas. Heat treated material in flowing HN 3 Reacting in gas for 26h to successfully prepare the CA-C block material.
The CA-C block material obtained in example 2 was subjected to a laser detonation test, which was carried out as follows:
the CA-C bulk material was placed on a metal cylinder. We chose a 1064nm laser, the laser power was controlled at 0.5W, and the beam was focused through a convex lens with a focal length of 10cm, illuminating the CA-C bulk material with a focal diameter of about 0.9 mm. The firing process was recorded using a high speed camera at 400000fps to investigate the laser response time, i.e. the time delay from laser exposure to the initiation point. The laser shines on the CA-C block material and at 16.1ms there is a large bright flame with a violent explosion and sound.
Claims (4)
1. The copper azide composite initiation explosive block material is characterized by being prepared by the following method:
(1) Preparation of precursor Material MOF-199 hybrid Material
Dissolving MOF-199 and sodium alginate in distilled water, and stirring until the mixture is uniformly dispersed; simultaneously, respectively dissolving polyacrylic acid and anhydrous calcium chloride in distilled water, and mixing the two solutions to obtain a solidified solution; dropping the sodium alginate dispersion liquid of the MOF-199 into the curing solution, washing with distilled water after the MOF-199 hybrid material is shaped, and drying;
(2) The method for preparing the CA-C bulk material comprises the following steps:
the resulting MOF-199 hybrid material was placed in a tube furnace, heat treated under nitrogen, and then placed over a flowing HN 3 Reacting in gas to prepare the copper azide composite initiating explosive block material.
2. The copper azide composite primary explosive block material of claim 1 wherein the different molds are used to mold the MOF-199 hybrid material in the desired shape during sizing.
3. The method for preparing the copper azide composite primary explosive block material according to claim 1, which is realized by the following steps:
(1) Preparation of precursor Material MOF-199 hybrid Material
Dissolving MOF-199 and sodium alginate in distilled water, and stirring until the mixture is uniformly dispersed; simultaneously, respectively dissolving polyacrylic acid and anhydrous calcium chloride in distilled water, and mixing the two solutions to obtain a solidified solution; dropping the sodium alginate dispersion liquid of the MOF-199 into the curing solution, washing with distilled water after the MOF-199 hybrid material is shaped, and drying;
(2) The method for preparing the CA-C bulk material comprises the following steps:
the resulting MOF-199 hybrid material was placed in a tube furnace, heat treated under nitrogen, and then placed over a flowing HN 3 Reacting in gas to prepare the copper azide composite initiating explosive block material.
4. The method for preparing copper azide composite initiating explosive block material according to claim 3, wherein in the step (1), different molds are used for molding the MOF-199 hybrid material with the required shape during the shaping.
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| CN116903426A (en) * | 2023-07-19 | 2023-10-20 | 郑州大学 | Rapid preparation method of copper azide composite initiating explosive |
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