CN110857215A - Method for preparing low-sensitivity copper azide from composite CNTs and copper nanowires - Google Patents
Method for preparing low-sensitivity copper azide from composite CNTs and copper nanowires Download PDFInfo
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Abstract
The invention discloses a method for preparing low-sensitivity copper azide from a composite carbon nano tube and a copper nano wire. The preparation method can effectively reduce the influence of external force on reaction products and improve the safety and reliability. Sodium azide and stearic acid are used as reactants, the adopted device is simple, and the azide efficiency is higher. The carbon material is utilized to reduce the accumulation of electrostatic charges on the composite material, thereby achieving the purpose of reducing the electrostatic sensitivity of copper azide without influencing the excellent initiation performance of the copper azide.
Description
Technical Field
The invention relates to the field of preparation of micro-nano energetic materials, in particular to a method for preparing low-sensitivity copper azide by using composite CNTs and copper nanowires.
Background
Copper azide is an extremely sensitive initiating explosive, the limit dosage required by the initiation of the Tylan is 0.4mg, and is one sixth of that of lead azide, so that the dosage can be greatly reduced, the safety of weapons can be improved, the input energy can be reduced, and the requirement of microminiature initiating explosive devices can be met. In addition, the copper ions belong to environment-friendly materials, and can reduce the generation of harmful substances and protect the environment compared with other heavy metal ions such as lead ions and the like. Copper azide, however, has been a strictly banned primary explosive due to its extremely high sensitivity. Therefore, how to reduce the sensitivity of copper azide and further optimize and improve the charge density, strength, sensitivity control, energy density control and the like is a problem to be solved.
In 2007, Jason et al prepared a copper azide initiation layer with nano-or micro-scale porosity and high consistency, compatible with MEMS processes. In 2014, petanhua, lina et al disclosed a method and apparatus for synthesizing copper azide. The problem of high risk during copper azide synthesis is solved, and a new process and a new technology are provided for the preparation of the novel green initiating explosive. In 2015, the second three kings of the warrior industry in china and the like adopt an in-situ reaction method to fill copper azide in a carbon nanotube array, adopt an electrochemical deposition method to fill nano-metallic copper in the wall of a carbon nanotube, and then utilize gas-solid in-situ reaction to obtain the carbon nanotube array filled with the copper azide. In 2016, Yangli, Beijing university of Physician, and the like, copper azide is filled into a carbonized metal organic framework, so that the sensitivity of the copper azide is greatly reduced, and the performances of the copper azide in all aspects are greatly improved.
The method has the advantages that the electrostatic insensitive carbon-copper azide composite energetic material is prepared by taking a copper-containing organic framework (MOFs) as a precursor through high-temperature carbonization and gas-solid azide reaction for the first time innovatively by the cooperation of Yankee teaching in an explosion focus laboratory of Beijing university of science and engineering and the Wangbo professor. The method gives full play to the structural characteristics of MOFs, and the arrangement of organic ligands and metal ions or clusters has obvious directionality, so that various frame pore structures are formed.
Disclosure of Invention
The invention aims to provide a method for preparing low-sensitivity copper azide by using a composite carbon nanotube and a copper nanowire.
The technical solution for realizing the purpose of the invention is as follows:
a method for preparing low-sensitivity copper azide from a composite carbon nano tube and a copper nano wire comprises the steps of preparing the copper nano wire by a liquid phase reduction method, mixing the copper nano wire with a single-wall carbon nano tube, depositing the prepared composite material on a conductive substrate by an electrochemical deposition method, and preparing the copper azide/carbon nano tube composite energetic material by a gas-solid phase azide reaction.
Furthermore, in the copper azide/carbon nano tube composite energetic material, the mass of the carbon nano tube is 3.0-15.0%.
The method specifically comprises the following steps:
step 1: preparing NaOH solution, cooling, adding into a three-neck flask, and sequentially adding Cu (NO) in sequence3)2Fully and uniformly mixing the solution, EDA and hydrazine hydrate solution;
step 2: placing the three-neck flask in a water bath for heating reaction, taking the three-neck flask out for cooling after the reaction is finished, centrifugally washing and collecting a product, and storing the obtained copper nanowire in absolute ethyl alcohol for later use;
and step 3: adding the copper nanowires into absolute ethyl alcohol mother liquor and adding the single-walled carbon nanotubes into SDS dispersion liquid, respectively carrying out ultrasonic treatment, mixing the absolute ethyl alcohol mother liquor of the copper nanowires with the carbon nanotube dispersion liquid, and uniformly stirring by magnetic force;
and 4, step 4: carrying out centrifugal washing and collection on the mixture obtained in the step (3), and carrying out vacuum drying to obtain the composite material of the copper nanowire and the single-walled carbon nanotube;
and 5: adding aluminum nitrate into a mixed solution of ethanol and acetone, dispersing into a uniform solution, adding the copper nanowire/single-walled carbon nanotube composite material into the dispersed uniform solution, performing ultrasonic dispersion and standing, and taking supernatant to obtain a stably dispersed electrophoresis solution;
step 6: taking a silicon substrate as a cathode and a graphite plate as an anode, adding the electrophoresis solution prepared in the step (5), drying, and forming a compact and uniform thin film on the silicon substrate;
and 7: and (3) in an inert atmosphere, adding a sodium azide aqueous solution into stearic acid to form hydrogen azide gas, and carrying out gas-solid phase azide reaction with the copper nanowire/single-walled carbon nanotube composite material deposited on the silicon substrate in the step (6) to obtain the copper azide/single-walled carbon nanotube composite energetic material.
Further, the concentration of NaOH solution is 10-20mol/mL, Cu (NO)3)2The concentration of the solution is 0.05-0.2mol/mL, the mass fraction of the hydrazine hydrate solution is 20% -40%, and the Cu (NO) is3)2The volume ratio of solution to EDA was 2: 1.
further, in the step 2, the water bath temperature of the three-neck flask is 70-90 ℃, and the reaction time is 1-2 h.
Further, in the step 3, the concentrations of the absolute ethyl alcohol mother liquor of the copper nanowire and the SDS dispersing liquid of the single-walled carbon nanotube are respectively 4-8mg/mL and 0.2-0.6mg/mL, the volume ratio is 0.35-0.65, the ultrasonic treatment time is 0.5-2h, the stirring time is 1-3h, the vacuum drying temperature is 50-70 ℃, and the vacuum drying time is 1-4 h.
Further, in step 5, the volume ratio of ethanol to acetone is 1: 2, the ultrasonic treatment time is 20min-40 min.
Further, the silicon substrate has a silicon wafer size of 30mm × 13mm × 0.2 mm.
Further, in the step 7, the gas-solid phase azidation reaction time is 48-72 h.
Compared with the prior art, the invention has the advantages that:
(1) the composite carbon nano tube and the copper nano wire are subjected to gas-solid phase nitridization reaction to prepare the copper nitridized/carbon nano tube composite energetic material, and the electrostatic sensitivity of the copper nitridized is reduced by adding the carbon nano tube.
(2) Sodium azide and stearic acid are used as reactants, the generated hydrogen azide gas further reacts with the copper nanowire, the reaction device is simpler and easier, the operation is convenient, and the reaction efficiency is greatly improved.
(3) The carbon nano tube and the copper nano wire are mixed to prepare the copper nano wire modified by the carbon nano tube, and the copper nano wire is subjected to electrophoretic deposition to obtain a compact and flat composite material film which is used for azidation and is safer and more efficient.
Drawings
FIG. 1 is an SEM image of copper nanowires in example 1 with EDA of 1.5 mL.
FIG. 2 is a TEM image of copper nanowires in example 1 with EDA amount of 1.5 mL.
Fig. 3 is an SEM image of the copper nanowire/carbon nanotube composite in example 1.
Fig. 4 is an XRD pattern of the copper nanowire/carbon nanotube composite in example 1.
Fig. 5 is an SEM image of the copper azide/carbon nanotube composite in example 1.
FIG. 6 is an SEM image of copper nanowires using EDA in an amount of 1.8mL in example 2.
FIG. 7 is a TEM image of copper nanowires using EDA in an amount of 1.8mL in example 3.
Fig. 8 is the XRD pattern of the carbon nanotube-based composite energetic material in example 2.
FIG. 9 is an SEM image of copper nanowires using EDA in an amount of 3.0mL in example 3.
FIG. 10 is TEM image of copper nanowire with EDA amount of 3.0mL in example 3.
Fig. 11 is a thermogram of the carbon nanotube-based composite energetic material in example 3.
FIG. 12 is a schematic diagram of the azide experimental apparatus in example 1.
Fig. 13 is a flow chart of the preparation of the copper azide/carbon nanotube composite energetic material in example 1.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments
As shown in fig. 13, the method firstly utilizes a liquid phase reduction method to prepare the copper nanowire, then mixes the copper nanowire with the single-walled carbon nanotube, deposits the prepared composite material on a conductive substrate by an electrochemical deposition method, and prepares the copper azide/carbon nanotube composite energetic material by a gas-solid phase azide reaction. The preparation device used in the invention is shown as 12.
In the following embodiments, the mass content of the carbon nanotube is preferably 3.0-15.0%, the volume of EDA in the preparation of the copper nanowire is preferably 0.5-4.5 mL, the water bath temperature is preferably 70-90 ℃, and the reaction time is preferably 1-2 h; the volume ratio of the absolute ethyl alcohol mother liquor of the copper nanowire to the carbon nanotube dispersion liquid is preferably 0.35-0.65, and the azide reaction time is preferably 48-72 h.
Example 1
Preparing 200mL NaOH solution with the concentration of 15mol/mL by using a volumetric flask, cooling, adding the NaOH solution into a 500mL three-neck flask, and sequentially adding Cu (NO) in sequence3)2Solution (10mL, 0.1mol/L), 1.5mL of EDA and hydrazine hydrate (0.25mL, 35 wt%) solution, mixing well; then placing the three-neck flask in a water bath, heating to 80 ℃, and reacting for 1 h; after the reaction is finished, taking out the three-neck flask, and cooling to room temperature; the product was centrifuged, washed with deionized water by centrifugation-redispersion and collected repeatedly several times. And storing the obtained copper nanowires in absolute ethyl alcohol for later use. Preparing 5mg/mL absolute ethyl alcohol mother liquor by using the copper nanowires, carrying out ultrasonic treatment for 30min for later use, and carrying out ultrasonic treatment on the single-walled carbon nanotube in an SDS solution for 30min to obtain a uniform dispersion liquid, wherein the concentration of the solution is 0.4 mg/mL; respectively mixing the absolute ethyl alcohol mother liquor of the copper nanowires and the carbon nanotube dispersion liquid according to the proportion of 1: 1, magnetically stirring for 2 hours, centrifugally separating for 5 minutes at the rotating speed of 7500r/min, repeatedly washing and collecting the mixture for several times by using deionized water in a centrifugal-redispersion mode, and drying the mixture for 24 hours at the temperature of 50 ℃ in vacuum to obtain the composite material of the copper nanowire and the single-walled carbon nanotube. Adding 10mL of ethanol and 20mL of acetone mixed solution into a 250mL beaker, and adding 2.4mg of aluminum nitrate; and adding 80mg of the copper nanowire/single-walled carbon nanotube composite material into the prepared solution, performing ultrasonic dispersion for 0.5h, standing for 10min, and taking supernatant to obtain the stably-dispersed electrophoretic solution. Taking a silicon substrate as a cathode and a graphite plate as an anode, adjusting the distance between the two electrodes to be 1cm, adding the prepared electrophoresis solution, applying a constant voltage of 25V by a computer, turning off a power supply after 20min, and taking out a sampleAnd (6) drying. Placing the copper nanowire/carbon nanotube composite material film into an azide device, and adding 1.0g of sodium azide (NaN)3) And 5.5g of stearic acid (C)18H36O2) And (3) putting the glass wool into a 250mL three-neck flask, introducing 15min of nitrogen, starting a magnetic stirrer, programming to 133 ℃, stopping heating after the generated ammonia gas and the copper nanowires placed on the glass wool fully react, and reacting for 48 hours. As can be seen from FIGS. 1 and 2, the prepared copper nanowires have uniform morphology and large length-diameter ratio. As can be seen from fig. 3, the single-walled carbon nanotubes are in a high-density transparent network and wrap the copper nanowires, indicating that the two are well combined together. The XRD pattern further proves the structural composition of the copper nanowire and the carbon nanotube. As can be seen from fig. 5, the carbon nanotubes are in a high-density transparent mesh, and the copper azide is coated to reduce energy accumulation and electrostatic sensitivity. Through an electrostatic sensitivity experiment, the 50% ignition energy of the composite material is 0.55mJ, which is obviously higher than the 50% electrostatic ignition energy (0.2mJ) of pure copper azide, and the sensitivity is improved.
Example 2
Preparing 200mL NaOH solution with the concentration of 15mol/mL by using a volumetric flask, cooling, adding the NaOH solution into a 500mL three-neck flask, and sequentially adding Cu (NO) in sequence3)2Solution (10mL, 0.1mol/L), 1.8mL of EDA and hydrazine hydrate (0.25mL, 35 wt%) solution, mixing well; then placing the three-neck flask in a water bath, heating to 85 ℃, and reacting for 1.5 h; after the reaction is finished, taking out the three-neck flask, and cooling to room temperature; the product was centrifuged, washed with deionized water by centrifugation-redispersion and collected repeatedly several times. And storing the obtained copper nanowires in absolute ethyl alcohol for later use. Preparing 5mg/mL absolute ethyl alcohol mother liquor by using the copper nanowires, carrying out ultrasonic treatment for 20min for later use, and carrying out ultrasonic treatment on the single-walled carbon nanotube in an SDS solution for 20min to obtain a uniform dispersion liquid, wherein the concentration of the solution is 0.4 mg/mL; respectively mixing the absolute ethyl alcohol mother liquor of the copper nanowires and the carbon nanotube dispersion liquid according to the proportion of 1: 2, magnetically stirring for 2 hours, centrifugally separating for 5min at the rotating speed of 7500r/min, repeatedly washing and collecting with deionized water in a centrifugal-redispersion mode for several times at 55 DEG CAnd (5) drying for 24h in vacuum to obtain the composite material of the copper nanowire and the single-walled carbon nanotube. Adding 10mL of ethanol and 20mL of acetone mixed solution into a 250mL beaker, and adding 2.4mg of aluminum nitrate; and adding 80mg of the copper nanowire/single-walled carbon nanotube composite material into the prepared solution, performing ultrasonic dispersion for 0.5h, standing for 10min, and taking supernatant to obtain the stably-dispersed electrophoretic solution. Taking a silicon substrate as a cathode and a graphite plate as an anode, adjusting the distance between the two electrodes to be 1cm, adding the prepared electrophoresis solution, applying a constant voltage of 25V by a computer, turning off a power supply after 20min, taking out a sample, and drying. Placing the copper nanowire/carbon nanotube composite material film into an azide device, and adding 1.0g of sodium azide (NaN)3) And 5.5g of stearic acid (C)18H36O2) And (3) putting the glass wool into a 250mL three-neck flask, introducing 15min of nitrogen, starting a magnetic stirrer, programming to 133 ℃, stopping heating after the generated ammonia gas and the copper nanowires placed on the glass wool fully react, and reacting for 60 hours. From fig. 6 and 7, it can be seen that the prepared copper nanowires have more uniform morphology and larger aspect ratio, but have individual larger copper particles, which is related to the addition amount of EDA. As can be seen from fig. 8, there is no characteristic diffraction peak of copper in the figure, which indicates that after the reaction is completed, copper is completely reacted, and the reaction product is cuprous azide/copper azide mixed crystal in which cuprous azide is the main component. Through an electrostatic sensitivity test, the 50% ignition energy of the composite material is 0.50mJ, which is higher than the 50% electrostatic ignition energy (0.2mJ) of pure copper azide, and the sensitivity is improved.
Example 3
Preparing 200mL NaOH solution with the concentration of 15mol/mL by using a volumetric flask, cooling, adding the NaOH solution into a 500mL three-neck flask, and sequentially adding Cu (NO) in sequence3)2Solution (10mL, 0.1mol/L), 3.0mL of EDA and hydrazine hydrate (0.25mL, 35 wt%) solution, mixing well; then placing the three-neck flask in a water bath, heating to 85 ℃, and reacting for 2.0 h; after the reaction is finished, taking out the three-neck flask, and cooling to room temperature; the product was centrifuged, washed with deionized water by centrifugation-redispersion and collected repeatedly several times. And storing the obtained copper nanowires in absolute ethyl alcohol for later use. Preparing the copper nano-wire into 5mg/mL of anhydrous BCarrying out ultrasonic treatment on the alcohol mother liquor for 20min for later use, and carrying out ultrasonic treatment on the single-walled carbon nanotube in an SDS solution for 20min to obtain a uniform dispersion liquid, wherein the concentration of the solution is 0.4 mg/mL; respectively mixing the absolute ethyl alcohol mother liquor of the copper nanowires and the carbon nanotube dispersion liquid according to the ratio of 2: 1, magnetically stirring for 1h, performing centrifugal separation for 5min at the rotating speed of 7500r/min, repeatedly washing and collecting the mixture for several times by using deionized water in a centrifugal-redispersion mode, and performing vacuum drying at 60 ℃ for 36h to obtain the composite material of the copper nanowire and the single-walled carbon nanotube. Adding 10mL of ethanol and 20mL of acetone mixed solution into a 250mL beaker, and adding 2.4mg of aluminum nitrate; and adding 80mg of the copper nanowire/single-walled carbon nanotube composite material into the prepared solution, performing ultrasonic dispersion for 0.5h, standing for 30min, and taking supernatant to obtain the stably-dispersed electrophoretic solution. Taking a silicon substrate as a cathode and a graphite plate as an anode, adjusting the distance between the two electrodes to be 1cm, adding the prepared electrophoresis solution, applying a constant voltage of 25V by a computer, turning off a power supply after 20min, taking out a sample, and drying. Placing the copper nanowire/carbon nanotube composite material film into an azide device, and adding 1.0g of sodium azide (NaN)3) And 5.5g of stearic acid (C)18H36O2) And (3) putting the glass wool into a 250mL three-neck flask, introducing 15min of nitrogen, opening a magnetic stirrer, programming to 133 ℃, stopping heating after the generated ammonia gas and the copper nanowires placed on the glass wool fully react, and reacting for 72 h. It can be seen from fig. 9 and 10 that the copper nanowires produced are more uniform in morphology, but there are individually larger copper particles, which is related to the amount of EDA added, and when the amount of EDA is more than 3mL, copper particles are produced. As can be seen from the DSC curve of FIG. 11, the exothermic reaction started at 168.3 deg.C, the termination temperature was 216.8 deg.C, the peak temperature was about 192.2 deg.C, and the heat evolution calculated by integrating the shaded portion of the exothermic peak curve was about 511.7mJ, thus the heat evolution of the product was about 1044.3J/g. The carbon nanotube-based composite energetic material prepared by the method has the advantages of advanced thermal decomposition temperature and higher heat release. Through an electrostatic sensitivity test, the 50% ignition energy of the composite material is 0.40mJ, which is higher than the 50% electrostatic ignition energy (0.2mJ) of pure copper azide, and the sensitivity is improved.
Claims (9)
1. A method for preparing low-sensitivity copper azide from composite CNTs and copper nanowires is characterized in that a liquid phase reduction method is used for preparing the copper nanowires, then the copper nanowires and single-walled carbon nanotubes are mixed, the prepared composite material is deposited on a conductive substrate by an electrochemical deposition method, and the copper azide/carbon nanotube composite energetic material is prepared through a gas-solid phase azide reaction.
2. The method of claim 1, wherein the copper azide/carbon nanotube composite energetic material comprises carbon nanotubes in an amount of 3.0% to 15.0% by mass.
3. The method according to claim 1, characterized in that it comprises in particular the steps of:
step 1: preparing NaOH solution, cooling, adding into a three-neck flask, and sequentially adding Cu (NO) in sequence3)2Fully and uniformly mixing the solution, EDA and hydrazine hydrate solution;
step 2: placing the three-neck flask in a water bath for heating reaction, taking the three-neck flask out for cooling after the reaction is finished, centrifugally washing and collecting a product, and storing the obtained copper nanowire in absolute ethyl alcohol for later use;
and step 3: adding the copper nanowires into absolute ethyl alcohol mother liquor and adding the single-walled carbon nanotubes into SDS dispersion liquid, respectively carrying out ultrasonic treatment, mixing the absolute ethyl alcohol mother liquor of the copper nanowires with the carbon nanotube dispersion liquid, and uniformly stirring by magnetic force;
and 4, step 4: carrying out centrifugal washing and collection on the mixture obtained in the step (3), and carrying out vacuum drying to obtain the composite material of the copper nanowire and the single-walled carbon nanotube;
and 5: adding aluminum nitrate into a mixed solution of ethanol and acetone, dispersing into a uniform solution, adding the copper nanowire/single-walled carbon nanotube composite material into the dispersed uniform solution, performing ultrasonic dispersion and standing, and taking supernatant to obtain a stably dispersed electrophoresis solution;
step 6: taking a silicon substrate as a cathode and a graphite plate as an anode, adding the electrophoresis solution prepared in the step (5), drying, and forming a compact and uniform thin film on the silicon substrate;
and 7: and (3) in an inert atmosphere, adding a sodium azide aqueous solution into stearic acid to form hydrogen azide gas, and carrying out gas-solid phase azide reaction with the copper nanowire/single-walled carbon nanotube composite material deposited on the silicon substrate in the step (6) to obtain the copper azide/single-walled carbon nanotube composite energetic material.
4. The method of claim 7, wherein the NaOH solution has a concentration of 10-20mol/mL, Cu (NO)3)2The concentration of the solution is 0.05-0.2mol/mL, the mass fraction of the hydrazine hydrate solution is 20% -40%, and the Cu (NO) is3)2The volume ratio of solution to EDA was 2: 1.
5. the method of claim 7, wherein in the step 2, the water bath temperature of the three-neck flask is 70-90 ℃, and the reaction time is 1-2 h.
6. The method of claim 7, wherein in step 3, the concentrations of the absolute ethyl alcohol mother liquor and the single-wall carbon nanotube SDS dispersion liquid of the copper nanowires are respectively 4-8mg/mL and 0.2-0.6mg/mL, the volume ratio is 0.35-0.65, the ultrasonic treatment time is 0.5-2h, the stirring time is 1-3h, the vacuum drying temperature is 50-70 ℃, and the time is 1h-4 h.
7. The method of claim 7, wherein in step 5, the volume ratio of ethanol to acetone is 1: 2, the ultrasonic treatment time is 20min-40 min.
8. The method of claim 7, wherein the silicon substrate has a wafer size of 30mm x 13mm x 0.2 mm.
9. The method of claim 7, wherein in step 7, the gas-solid phase azidation reaction is carried out for a period of time of 48h to 72 h.
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| CN115536483A (en) * | 2022-10-24 | 2022-12-30 | 北京理工大学 | Copper azide energetic film and preparation method thereof |
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