CN112643025A - Preparation method of high-reactivity nano aluminum/copper oxide microspheres - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C—CHEMISTRY; METALLURGY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a preparation method of a high-reactivity nano aluminum/copper oxide microsphere, which comprises the following steps of firstly, adding a binder into a benign organic solvent, magnetically stirring at room temperature to fully dissolve the binder, then respectively adding weighed nano Al and nano CuO, magnetically stirring, performing ultrasound, and finally stirring the solution after the ultrasound to obtain Al precursor solution and CuO precursor solution; injecting two prepared precursor solutions into a disposable injector, wherein Al precursor solution is communicated with an inner tube, and CuO precursor solution is communicated with an outer tube; and thirdly, scraping the composite particles on the aluminum foil of the collecting plate, and drying the composite particles in a freeze dryer to obtain the nano Al/CuO composite particles. The nano CuO particles prepared by the method are dispersed and coated in the microspheres, so that the technical problems of energy density and easy oxidation of metal aluminum powder after the nano aluminum powder is coated by the traditional method are solved.
Description
Technical Field
The invention relates to a preparation method of a high-reactivity nano aluminum/copper oxide microsphere, in particular to the field of preparation of a nano Al/CuO microsphere.
Background
The Metastable Intermolecular Complex (MIC) is a nanoscale metal-based reaction material compounded by nanoscale fuel and oxidant, and may also be referred to as a nano thermite. The metastable state intermolecular compound has the advantages of high volume energy density, high reaction temperature, fast energy release rate, high reaction heat value, low ignition initiation energy, easy preparation and the like, and the combustion performance of the nano thermite can be controlled and changed by adjusting components, equivalent ratio and particle size. The nano thermite is widely applied to civil and military fields due to the excellent heat release and combustion characteristics of the nano thermite. Because the preparation process adopted by the nano thermite has good compatibility with the preparation process of a Micro Electro Mechanical System (MEMS) device, the nano thermite film can be integrated into the MEMS device to form an MEMS energetic ignition device; due to the excellent high-reaction thermal property, the MIC can be applied to many fields, including micro-ignition, rapid initiation, material processing, micro-power generation and the like; the gases released in the reaction are relevant to the application fields, including micro-driving, micro-propelling, gas generators and the like; meanwhile, as a high-energy additive, the composite material also has wide application prospect in solid propellants.
Enayati et al encapsulation efficiency of 65-75% of loaded PLGA microparticles prepared by co-axial electrospray (Enayati, Marjan, et al, "One-step electrophoretic production of drug-loaded micro-and nanoparticles," Journal of the Royal Society Interface 7.45(2009):667 cake 675.); xie et al (PLGA) microparticles prepared by coaxial electrospray, with encapsulated lytic enzymes having a biological activity higher than 90% and encapsulated bovine whey protein (BSA) sustained release for up to 30 days in vitro experiments, the coaxial electrospray process effectively protected the biological activity of the drug by encapsulating it in the core layer (Xie, Jingweni, et al. "Encapsulation of protein drugs in bipolar microparticles by co-axial electrospray." Journal of colloidal and interfacial science 317.2(2008): 469-476.); he and the like synthesize polydopamine on the surface of aluminum powder by an in-situ synthesis method, and then prepare a core-shell structure of Al @ PDA @ CuO, wherein the thermite prepared by the method has excellent heat release performance, but the dopamine non-energetic component synthesized in the method reduces the energy density of an MIC material (He, Wei, et Al. "Mussel-embedded polypyamine-direct crystal growth of core-shell n-Al @ PDA @ CuO metallic mixed compositions." Chemical Engineering Journal 369 2019: (1093) -; wang et Al prepared Al/CuO microspheres by uniaxial electrostatic spraying, and accurately regulated the size of the microspheres by changing the content of binder Nitrocotton (NC). The CuO/Al nano thermite prepared by the method has the advantages of close contact among components, high purity, adjustable size, excellent Combustion performance and the like, but cannot form a core-shell structure of Al @ CuO and cannot effectively solve the problem that nano aluminum is easy to oxidize (Wang, Haiyang, et Al. "Assembly and reactive properties of Al/CuO based nano thermal polymers." Combustion and Flame 161.8(2014): 2203-2208.).
At present, relevant reports about coaxial electrospray mainly focus on wrapping biomacromolecule and hydrophobic micromolecule drugs such as deoxynucleotide, protein, budesonide and the like, and relatively few researches are carried out on micro-nano composite energetic materials.
Disclosure of Invention
The invention aims to provide a preparation method of a nano aluminum/copper oxide microsphere with high reactivity.
The technical solution for realizing the purpose of the invention is as follows:
the preparation method of the nano aluminum/copper oxide microsphere with high reactivity comprises the following steps
Firstly, adding a binder into a benign organic solvent, carrying out magnetic stirring at room temperature to fully dissolve the binder, then respectively adding weighed nano Al and nano CuO, carrying out magnetic stirring and ultrasonic treatment, and finally stirring the ultrasonic solution to obtain Al precursor solution and CuO precursor solution;
step two, injecting the two prepared precursor solutions into a disposable injector, wherein Al precursor solution is communicated with an inner tube, CuO precursor solution is communicated with an outer tube,
and thirdly, scraping the composite particles on the aluminum foil of the collecting plate, and drying the composite particles in a freeze dryer to obtain the nano Al/CuO composite particles.
Furthermore, the inner diameter of the coaxial nozzle needle is 0.41mm, and the outer diameter of the coaxial nozzle needle is 0.72 mm.
Further, the solution was magnetically stirred for 10 minutes, sonicated for 1 hour, and finally the sonicated solution was stirred for 24 hours.
Further, the injection amount of the disposable syringe was 5 ml.
And step three, the injection speed of the inner tube of the disposable injector is 0.18mm/min, and the injection speed of the outer tube is 0.23 mm/min.
Furthermore, the distance between the needle head of the disposable syringe and the collecting plate is 10cm, the positive voltage is 8-10 KV, and the negative voltage is-3 KV.
Compared with the prior art, the invention has the following remarkable advantages: 1. the nanometer thermite microspheres are prepared by adopting a coaxial electrostatic spraying method, the sphericity of the microspheres is high, the particle size distribution is uniform, and the microspheres are not easy to agglomerate. The energy-containing component Nitrocotton (NC) tightly connects the single nano Al and nano CuO particles together, thereby effectively avoiding the agglomeration of nano aluminum powder. 2. The components are contacted compactly, so that the mass transfer distance is shortened, and the reaction performance is greatly improved. 3. The nano CuO particles are dispersed and coated in the microspheres, so that the technical problems of energy density and easy oxidation of metal aluminum powder after the nano aluminum powder is coated by the traditional method are solved to a certain extent.
Drawings
FIG. 1 is SEM image of nano Al/CuO.
FIG. 2 EDS diagram of nano Al/CuO.
FIG. 3 is a DSC curve diagram of nano Al/CuO microspheres.
FIG. 4 SEM image of nano Al/CuO.
FIG. 5 SEM image of nano Al/CuO.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
A preparation method of a high-reactivity nano aluminum/copper oxide microsphere comprises the steps of firstly placing Al precursor liquid (nuclear layer) and CuO precursor liquid (shell layer) through magnetic stirring, an ultrasonic cleaning machine and the like, then respectively filling the precursor liquids into two independent injectors, then connecting the injectors into an inner pipe and an outer pipe of a nozzle, respectively propelling the liquids at a certain flow rate by connecting a high-voltage power supply, and finally collecting a sample on an aluminum foil.
The method comprises the following specific steps:
firstly, respectively adding 6mg and 18mg of binder nitrocotton into 2ml and 3ml of organic solvent acetone, magnetically stirring at room temperature to fully dissolve the binder nitrocotton, then respectively adding 200mg of nano Al powder and 600mg of nano CuO, magnetically stirring for 10 minutes, then performing ultrasonic treatment for 1 hour, and finally stirring the solution after ultrasonic treatment for 24 hours to obtain Al precursor solution (nuclear layer) and CuO precursor solution (shell layer);
injecting the two prepared precursor liquids into a 5ml disposable injector, wherein the Al precursor liquid is communicated with an inner tube, the CuO precursor liquid is communicated with an outer tube, the injection speed of the inner tube is 0.18mm/min, and the injection speed of the outer tube is 0.23 mm/min; the distance between the needle head and the collecting plate is 10cm, the positive voltage is 8-10 KV, and the negative voltage is-3 KV;
scraping the composite particles on the aluminum foil of the collecting plate, and drying in a freeze dryer to obtain nano Al/CuO composite particles;
example 1
Weighing 200mg of nano aluminum powder, 600mg of copper oxide and 6mg and 18mg of nitrocotton at room temperature, weighing 2mL and 3mL of solvent acetone, respectively putting the weighed nitrocotton into the weighed acetone at 25 ℃, and performing magnetic stirring at the speed of 500rpm to completely dissolve the nitrocotton, putting the weighed nano aluminum powder and the copper oxide into a nitrocotton solution, performing ultrasonic treatment at the ultrasonic frequency of 50kHZ for one hour, and performing magnetic stirring for 24 hours for later use. The obtained aluminum powder solution is quickly filled into a 10mL plastic syringe, a copper oxide solution is quickly filled into a 5mL plastic syringe, the 10mL plastic syringe is replaced by a 21G flat-top dispensing metal coaxial needle head, simultaneously, the copper oxide solution is introduced into an outer tube, then the syringe is arranged on a propulsion pump in an electrostatic spraying device with the environment temperature of 25 ℃, the flow rate of an inner tube propulsion pump is set to be 0.18mm/min, the flow rate of an outer tube propulsion pump is set to be 0.23mm/min, and positive high pressure is connected to a metal flat-top needle head. An aluminum foil as a collector was fixed to an insulating flat plate and connected to a negative high voltage power supply. The distance from the flat-top needle to the collector was adjusted to 10 cm. And opening a switch of the propulsion pump, firstly adjusting the negative voltage to-3 kV, then adjusting the positive voltage to 8kV, and enabling the metal needle head to have a Taylor cone. And (5) closing the instrument after stabilizing for a period of time to obtain the nano Al/CuO microspheres. FIG. 1 is a scanning electron micrograph of the nano Al/CuO microspheres obtained according to this example of 15000 times, and the particle size is about 3 μm. FIG. 2 is EDS diagram of nano Al/CuO microsphere. FIG. 3 is a differential scanning calorimetry curve of a nano Al/CuO sample prepared by a coaxial electrostatic spray method, and the heat release of the sample obtained by software integration is 1756J/g, which is 532J/g higher than that of a physical mixed sample.
Example 2
Weighing 200mg of nano aluminum powder, 600mg of copper oxide and 12mg and 36mg of nitrocotton at room temperature, weighing 2mL and 3mL of solvent acetone, respectively putting the weighed nitrocotton into the weighed acetone at 25 ℃, and performing magnetic stirring at the speed of 500rpm to completely dissolve the nitrocotton, putting the weighed nano aluminum powder and the copper oxide into a nitrocotton solution, performing ultrasonic treatment at the ultrasonic frequency of 50kHZ for one hour, and performing magnetic stirring for 24 hours for later use. The obtained aluminum powder solution is quickly filled into a 10mL plastic syringe, a copper oxide solution is quickly filled into a 5mL plastic syringe, the 10mL plastic syringe is replaced by a 21G flat-top dispensing metal coaxial needle head, simultaneously, the copper oxide solution is introduced into an outer tube, then the syringe is arranged on a propulsion pump in an electrostatic spraying device with the environment temperature of 25 ℃, the flow rate of an inner tube propulsion pump is set to be 0.18mm/min, the flow rate of an outer tube propulsion pump is set to be 0.23mm/min, and positive high pressure is connected to a metal flat-top needle head. An aluminum foil as a collector was fixed to an insulating flat plate and connected to a negative high voltage power supply. The distance from the flat-top needle to the collector was adjusted to 10 cm. And opening a switch of the propulsion pump, firstly adjusting the negative voltage to-3 kV, then adjusting the positive voltage to 10kV, and enabling the metal needle head to have a Taylor cone. And (5) closing the instrument after stabilizing for a period of time to obtain the nano Al/CuO microspheres. FIG. 4 is scanning electron micrographs of 10000 times and 50000 times of nano Al/CuO microspheres obtained according to this example, and the sphericity of the particles is relatively low. It can be seen that with the increase of the concentration of the nitrocotton, the sample has a random shape, and composite particles with better spherical degree are difficult to form. In the process of solvent volatilization, excessive nitrocotton can make Al and CuO difficult to assemble into spherical particles, but because the nitrocotton has good cohesiveness, Al and CuO are still combined compactly, so that the mass and heat transfer distance during the reaction is reduced, and the heat release performance of reactants is greatly improved.
Example 3
Weighing 200mg of nano aluminum powder, 800mg of copper oxide and 12mg and 36mg of nitrocotton at room temperature, weighing 2mL and 3mL of solvent acetone, respectively putting the weighed nitrocotton into the weighed acetone at 25 ℃, and performing magnetic stirring at 500rpm to completely dissolve the nitrocotton, putting the weighed nano aluminum powder and the copper oxide into a nitrocotton solution, performing ultrasonic treatment at an ultrasonic frequency of 50kHZ for one hour, and performing magnetic stirring for 24 hours for later use. The obtained aluminum powder solution is quickly filled into a 10mL plastic syringe, a copper oxide solution is quickly filled into a 5mL plastic syringe, the 10mL plastic syringe is replaced by a 21G flat-top dispensing metal coaxial needle head, simultaneously, the copper oxide solution is introduced into an outer tube, then the syringe is arranged on a propulsion pump in an electrostatic spraying device with the environment temperature of 25 ℃, the flow rate of an inner tube propulsion pump is set to be 0.18mm/min, the flow rate of an outer tube propulsion pump is set to be 0.23mm/min, and positive high pressure is connected to a metal flat-top needle head. An aluminum foil as a collector was fixed to an insulating flat plate and connected to a negative high voltage power supply. The distance from the flat-top needle to the collector was adjusted to 10 cm. And opening a switch of the propulsion pump, firstly adjusting the negative voltage to-3 kV, then adjusting the positive voltage to 8kV, and enabling the metal needle head to have a Taylor cone. And (5) closing the instrument after stabilizing for a period of time to obtain the nano Al/CuO microspheres. FIG. 5 is scanning electron micrographs of 5000 times, 10000 times and 50000 times of nano Al/CuO microspheres obtained according to the embodiment. It can be seen that although the stoichiometric ratio of reactants is changed, the coaxial electrostatic spraying can still prepare the reaction microspheres with higher sphericity under the condition of appropriate nitrocotton content. Meanwhile, a large amount of copper oxide nanoparticles exist on the surface of the microsphere, so that the contact area of the copper oxide nanoparticles and Al can be increased, and the problem that Al in the microsphere is easy to oxidize can be solved to a certain extent.
Claims (6)
1. The preparation method of the nano aluminum/copper oxide microspheres with high reactivity is characterized by comprising the following steps
Firstly, adding a binder into a benign organic solvent, carrying out magnetic stirring at room temperature to fully dissolve the binder, then respectively adding weighed nano Al and nano CuO, carrying out magnetic stirring and ultrasonic treatment, and finally stirring the ultrasonic solution to obtain Al precursor solution and CuO precursor solution;
step two, injecting the two prepared precursor solutions into a disposable injector, wherein Al precursor solution is communicated with an inner tube, CuO precursor solution is communicated with an outer tube,
and thirdly, scraping the composite particles on the aluminum foil of the collecting plate, and drying the composite particles in a freeze dryer to obtain the nano Al/CuO composite particles.
2. The method for preparing high-reactivity nano aluminum/copper oxide microspheres according to claim 1, wherein: the inner diameter of the coaxial nozzle needle is 0.41mm, and the outer diameter of the coaxial nozzle needle is 0.72 mm.
3. The method for preparing high-reactivity nano aluminum/copper oxide microspheres according to claim 1, wherein: magnetically stirring for 10 min, further sonicating for 1 hr, and finally stirring the sonicated solution for 24 hr.
4. The method for preparing high-reactivity nano aluminum/copper oxide microspheres according to claim 1, wherein: the injection amount of the disposable syringe was 5 ml.
5. The method for preparing high-reactivity nano aluminum/copper oxide microspheres according to claim 1, wherein: and step three, the injection speed of the inner tube of the disposable injector is 0.18mm/min, and the injection speed of the outer tube is 0.23 mm/min.
6. The method for preparing high-reactivity nano aluminum/copper oxide microspheres according to claim 1, wherein: and step three, the distance between the needle head of the disposable syringe and the collecting plate is 10cm, the positive voltage is 8-10 KV, and the negative voltage is-3 KV.
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Cited By (3)
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| CN114406271A (en) * | 2022-01-20 | 2022-04-29 | 山东省科学院新材料研究所 | Macroscopic preparation method, device and application of nanocarbon material-metal composite material |
| CN115819169A (en) * | 2022-12-15 | 2023-03-21 | 西安近代化学研究所 | Preparation method and application of Al/PVDF/MOx multi-shell structure composite energetic material |
| CN116332709A (en) * | 2023-02-22 | 2023-06-27 | 西安近代化学研究所 | Al/polyborane energetic composite material, preparation method and application |
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