CN105689724B - A kind of preparation method of nanometer of Al/CuO AP compound particles containing energy - Google Patents
A kind of preparation method of nanometer of Al/CuO AP compound particles containing energy Download PDFInfo
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- CN105689724B CN105689724B CN201610070127.XA CN201610070127A CN105689724B CN 105689724 B CN105689724 B CN 105689724B CN 201610070127 A CN201610070127 A CN 201610070127A CN 105689724 B CN105689724 B CN 105689724B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses the preparation method of a kind of nanometer of Al/CuO AP compound particles containing energy, comprise the following steps：(1) preparation of nanometer CuO particle；(2) nanometer Al/CuO preparation；(3) preparation of the AP solution of the Al/CuO containing nanometer；(4) preparation of nanometer Al/CuO AP compound particles.The method of the invention is in one layer of AP of thermite nanometer Al/CuO Surface coatings, improve AP and Al Nanoparticles, CuO contact area, promote AP decomposition, at the same using AP decompose caused by gas improve reaction system pressure, improve Al Nanoparticles and the heat and mass transport process of CuO reactions, strengthen it and contain and can show, the preparation method effectively solves the slow problem of reaction rate between thermite component, and preparation process is easy to operate, simple and safe, cost is low, suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of Energetic Nanomaterials, and in particular to a kind of nanometer Al/CuO-AP contains can be multiple
Close the preparation method of particle.
Background technology
Energetic Nanomaterials are more and more closed due to low initial reaction temperature, activation energy, and high burn rate
Note.Typically it is made up of the nano particle and matrix of metal/metal oxide and/or inorganic/organic energetic material component.Metal powder
Because that can increase energy, improve the advantages that quick-fried heat and capacity for work, improvement ignition performance, obtained in energetic material extensive
Using.And Al powder due to its excellent heat release and low-temperature oxidation ability and materials are abundant, cost is relatively low the advantages that, containing energy
Played an important role in Material Field.And the particle diameter of Al powder is smaller, specific surface area is bigger, and specific surface energy is higher, grand
See and can show new, excellent performance on microcosmic.Thermite such as MoO based on nanometer aluminium powder3/Al、Al/Fe2O3、
Al/CuO etc. presents the advantages that higher energy density and energy rate of release, but its reaction rate is limited by mass transport process
System.In order to improve the burn rate of energetic material, mass-and heat-transfer speed is a kind of effective method during strengthen burning.Shen
Deng (Shen, J., Qiao, Z., Wang, J., Zhang, K., Li, R., Nie, F., ＆ Yang, G.Combustion and
Flame,2014,161:2975-2981.) CL-20 is added in Al-CuO energetic materials, as a result shows, CL-20 is added into aluminium
After thermit powder, help lend some impetus to burning, compound particle combustion flame area is bigger, burn rate faster, show to add after CL-20
It is highly beneficial for thermite combustion process.
Ammonium perchlorate (AP) due to its oxygen content is high, without heavy metal ion, have high thermal stability and chemical stability,
And stable gaseous product can be completely converted into after cheap, simple production process, burning, extensive pass is obtained always
Note.
Research shows, and Al powder (the prosperous Push Technologies of Ma Zhenye, Li Fengsheng, Chen Aisi, Song Hong, 2004,25:373-376.)
With CuO (Hong Qin, Mingxia Zha, Zhenye Ma, Fengqi Zhao, Siyu Xu, Huixiang
Xu.Propellants Explosives Pyrotechnics,2014,39:694-700.) thermal decomposition for AP has one
Fixed catalytic action, and the two is the usual component of thermite.There is not yet high-purity nm Al/CuO-AP is compound in existing literature
The report of particle, and reported that the preparation technology of compound particle is complicated, it is difficult to a large amount of productions.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, methods described is adopted
With solvent evaporated method in one layer of AP of thermite Al/CuO Surface coatings, by AP addition Al/CuO systems, raising or enhancing AP and Al
The contact area of powder, CuO, contributes to AP decomposition, reduces AP decomposition temperatures, at the same the mass transfer of REINFORCED Al powder and CuO reactions with
Diabatic process, the slow problem of reaction rate between thermite component is efficiently solved, strengthen the mass-and heat-transfer speed of energy-containing particle；
Described preparation method is easy to operate, simple and safe, and cost is low.
Put it briefly, the preparation method of the nanometer Al/CuO-AP of the invention compound particle containing energy includes following four step：
The preparation of nanometer CuO particle；The preparation of Al/CuO energetic materials；The preparation of the AP solution of the Al/CuO containing nanometer；Nanometer Al/CuO-
The preparation of AP compound particles.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, comprises the following steps：
(1) preparation of nanometer CuO particle：
By Cu (NO3)2Or its hydrate adds DMAC (dimethyl acetamide) and H2O in the mixed solvent heating；By NaOH
Add DMAC and H as hereinbefore2O in the mixed solvents are warming up to mutually synthermal, and NaOH solution then is added into Cu (NO3)2
Reacted in solution, reaction product is filtered, washs, dries, and obtains nanometer CuO particle；
(2) nanometer Al/CuO preparation；
It is anti-that nanometer CuO prepared by step (1) is added to ultrasound in the aqueous isopropanol containing PVP (polyvinylpyrrolidone)
Should, through centrifuging, wash, the nanometer CuO of PVP modifications is obtained after drying, the nanometer CuO that foregoing PVP is modified and Al Nanoparticles are added
Enter ultrasonic reaction in isopropanol, centrifugation, washing, dry, obtain a nanometer Al/CuO；
(3) preparation of the AP solution of the Al/CuO containing nanometer；
Nanometer Al/CuO ultrasonic disperses prepared by step (2) obtain Al/CuO containing nanometer into the organic solvent containing AP
AP solution；
(4) preparation of nanometer Al/CuO-AP compound particles:
The AP solution for the Al/CuO containing nanometer that step (3) is obtained is added in rotary evaporator, is obtained after rotary evaporation
Nanometer Al/CuO-AP compound particles containing energy.
Cu (NO in the step (1)3)2It is preferably 1 with NaOH mol ratios:2~1:3.
DMAC and H in the step (1)2O in the mixed solvents DMAC and H2O volume ratio is preferably 3:1~5:1.
Reaction temperature is preferably 80 DEG C~110 DEG C in the step (1).
The reaction time is preferably 1~10min in the step (1).
The dosage of nanometer CuO is preferably isopropanols of the 0.10g~0.15g/200~300ml containing PVP in the step (2)
Solution.
PVP concentration is preferably 0.05%~0.15% (W/ in the aqueous isopropanol containing PVP described in the step (2)
V)。
The ultrasonic reaction time that the nanometer CuO of PVP modifications is prepared in the step (2) is preferably 4~5h.
The nanometer CuO and the mol ratio of Al Nanoparticles that PVP is modified in the step (2) are preferably 1.0~1.8：1.
The ultrasonic reaction time that nanometer Al/CuO is prepared in the step (2) is preferably 1~1.5h.
Nanometer Al/CuO quality is preferably 0.25~4 times of AP mass in the step (3).
Organic solvent described in the step (3) is preferably ethanol or acetone.
The ultrasonic disperse time is preferably 10~25min in the step (3).
Rotating evaporation temperature is preferably 10~30 DEG C in the step (4).
Rotary evaporator rotating speed is preferably 100~140rpm in the step (4).
The rotary evaporation time is preferably 10~25min in the step (4).
Beneficial effects of the present invention：
The preparation method of the nanometer Al/CuO-AP of present invention compound particles containing energy is in situ to nanometer Al/CuO straight from AP
It is compound to tap into row, is effectively improved AP and Al Nanoparticles, the contact area of nanometer CuO, while has facilitation to AP decomposition,
And AP decompose caused by gas be advantageous to improve reaction system pressure, enhancing Al Nanoparticles and nanometer CuO reaction mass transfer with
Diabatic process.The preparation process of compound particle is easy to operate, and preparation technology simplifies, and this method can be promoted for other compound containing energy
The preparation of particle, and it is adapted to large-scale production.The present invention specifically includes advantages below：
1) compound particle is prepared using solvent evaporated method, preparation process is easy to operate, simple and safe, and cost is low, Er Qieyou
It is only the volatilization of solvent present in preparation process, nanometer Al/CuO supplies AP in its superficial growth as nucleus, not shadow
The structure and changes of contents of each component into compound particle are rung, and in preparation process and is not introduced into other impurities, product is pure
Degree is high.
2) be advantageous to improve AP and Al Nanoparticles, the contact area of nanometer CuO, catalysis of both promotions to AP, reduce AP
Decomposition temperature, be advantageous to the progress of reaction.
3) by nanometer Al/CuO and AP Combined Processings, while AP decomposition temperatures are reduced, AP can be made full use of to decompose
Caused gas improves reaction system pressure, promotes Al Nanoparticles and the heat and mass transport of nanometer CuO reaction, may be very
Strengthen the combustibility and exothermicity of thermite in big degree.
With reference to specific embodiment, the present invention will be described in detail.Protection scope of the present invention is not with specific implementation
Mode is limited, but is defined in the claims.
Brief description of the drawings
The XRD of nanometer Al/CuO-AP prepared by Fig. 1 embodiments 1 compound particle containing energy.
The SEM figures of nanometer Al/CuO-AP prepared by Fig. 2 embodiments 1 compound particle containing energy.
Embodiment
Embodiment 1
The preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, comprises the following steps：
(1) preparation of nanometer CuO：By 1.457g Cu (NO3)2·3H2O adds 40ml DMAC and H2O volume ratios are 5：1
Mixed solution in be warming up to 100 DEG C, 0.5g NaOH are added to the DMAC and H of 20ml as hereinbefore2O mixed solution
In be warming up to 100 DEG C, NaOH solution is then quickly adding into Cu (NO3)2·3H2In O solution, there is substantial amounts of black to sink at once
Form sediment generation, react 5min after, will precipitate it is filtered, wash, be drying to obtain nanometer CuO.
(2) nanometer Al/CuO preparation：Weigh the nanometer CuO prepared in 0.10g steps (1) and be added to 200ml containing 0.1%
(W/V) ultrasonic 4h in PVP isopropanol, through centrifuging, washing, drying can obtain the nanometer CuO particles of PVP modifications.Then according to rubbing
You are than being 1:The 1 accurate nanometer CuO particle for weighing the above-mentioned PVP modifications of 0.1g adds ultrasound in 1.5ml isopropanols with Al Nanoparticles
1h is reacted, centrifugation, washing, in triplicate, is dried to obtain a nanometer Al/CuO.
(3) preparation of the AP solution of the Al/CuO containing nanometer：Take the nanometer Al/CuO prepared in 0.1g steps (2) to add to contain
In 0.15g AP acetone, ultrasonic disperse 10min, the AP solution of the Al/CuO containing nanometer is obtained.
(4) preparation of nanometer Al/CuO-AP compound particles:The AP solution for the Al/CuO containing nanometer that step (3) is obtained adds
Enter into rotary evaporator, above-mentioned solution is handled in 15 DEG C, 140rpm, after question response carries out 15min, on wall
To nanometer Al/CuO-AP compound particles.
XRD, FESEM are as depicted in figs. 1 and 2.As a result display contains energy compound particle largely particle spherical in shape, component crystal formation
Structural integrity.
Embodiment 2
The preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, comprises the following steps：
(1) preparation of nanometer CuO：By 1.457g Cu (NO3)2·3H2O adds 40ml DMAC and H2O volume ratios are 5：1
Mixed solution in be warming up to 90 DEG C, 0.5g NaOH are added to the DMAC and H of 20ml as hereinbefore2In O mixed solution
90 DEG C are warming up to, NaOH solution is then quickly adding into Cu (NO3)2·3H2In O solution, there is substantial amounts of black precipitate to give birth at once
Into, react 10min after, will precipitate it is filtered, wash, be drying to obtain nanometer CuO.
(2) nanometer Al/CuO preparation：Weigh the nanometer CuO prepared in 0.15g steps (1) and be added to 300ml containing 0.1%
(W/V) ultrasonic 4h in PVP isopropanol, through centrifuging, washing, drying can obtain the nanometer CuO particles of PVP modifications.Then according to rubbing
You are than being 1:The 1.8 accurate nanometer CuO particles for weighing the above-mentioned PVP modifications of 0.12g add ultrasound in 2ml isopropanols with Al Nanoparticles
1h is reacted, centrifugation, washing, in triplicate, is dried to obtain a nanometer Al/CuO.
(3) preparation of the AP solution of the Al/CuO containing nanometer：Take the nanometer Al/CuO prepared in 0.23g steps (2) to add to contain
In 0.15g AP acetone, ultrasonic disperse 10min, the AP solution of the Al/CuO containing nanometer is obtained.
(4) preparation of nanometer Al/CuO-AP compound particles:The AP solution for the Al/CuO containing nanometer that step (3) is obtained adds
Enter into rotary evaporator, above-mentioned solution is handled in 10 DEG C, 100rpm, after question response carries out 20min, on wall
To nanometer Al/CuO-AP compound particles.
Embodiment 3
The preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, comprises the following steps：
(1) preparation of nanometer CuO：By 1.457g Cu (NO3)2·3H2O adds 40ml DMAC and H2O volume ratios are 5：1
Mixed solution in be warming up to 110 DEG C, 0.5g NaOH are added to the DMAC and H of 20ml as hereinbefore2O mixed solution
In be warming up to 110 DEG C, NaOH solution is then quickly adding into Cu (NO3)2·3H2In O solution, there is substantial amounts of black to sink at once
Form sediment generation, react 10min after, will precipitate it is filtered, wash, be drying to obtain nanometer CuO.
(2) preparation of Al/CuO energetic materials：Weigh the nanometer CuO prepared in 0.12g steps (1) and be added to 250ml and contain
Ultrasonic 5h in 0.1% (W/V) PVP isopropanol, through centrifuging, washing, drying can obtain the nanometer CuO particles of PVP modifications.Then press
It is 1 according to mol ratio:The 1.6 accurate nanometer CuO particles for weighing the above-mentioned PVP modifications of 0.10g add 1.5ml isopropanols with Al Nanoparticles
Middle ultrasonic reaction 1.5h, centrifugation, washing, in triplicate, is dried to obtain a nanometer Al/CuO.
(3) preparation of the AP solution of the Al/CuO containing nanometer：Take the nanometer Al/CuO prepared in 0.038g steps (2) to add to contain
In 0.15g AP acetone, ultrasonic disperse 10min, the AP solution of the Al/CuO containing nanometer is obtained.
(4) preparation of nanometer Al/CuO-AP compound particles:The AP solution for the Al/CuO containing nanometer that step (3) is obtained adds
Enter into rotary evaporator, above-mentioned solution is handled in 30 DEG C, 120rpm, after question response carries out 25min, on wall
To nanometer Al/CuO-AP compound particles.
Through characterizing, nanometer Al/CuO-AP prepared by embodiment 2 and embodiment 3 containing can compound particle, its XRD, FESEM with
Fig. 1 and Fig. 2 are substantially similar.
Claims (8)
1. the preparation method of a kind of nanometer of Al/CuO-AP compound particles containing energy, comprises the following steps：
(1) preparation of nanometer CuO particle：
By Cu (NO3)2Or its hydrate adds DMAC and H2O in the mixed solvent heating；NaOH is added as hereinbefore
DMAC and H2O in the mixed solvents are warming up to mutually synthermal, and NaOH solution then is added into Cu (NO3)2React, react in solution
Product is filtered, washs, dries, and obtains nanometer CuO particle；
(2) nanometer Al/CuO preparation；
Nanometer CuO prepared by step (1) is added to ultrasonic reaction in the aqueous isopropanol containing PVP, through centrifuging, washing, dry
The nanometer CuO of PVP modifications is obtained afterwards, the nanometer CuO that foregoing PVP is modified adds ultrasonic reaction in isopropanol with Al Nanoparticles,
Centrifugation, washing, dry, obtain a nanometer Al/CuO；
(3) preparation of the AP solution of the Al/CuO containing nanometer；
Nanometer Al/CuO ultrasonic disperses prepared by step (2) obtain the AP of the Al/CuO containing nanometer into the organic solvent containing AP
Solution；
(4) preparation of nanometer Al/CuO-AP compound particles:
The AP solution for the Al/CuO containing nanometer that step (3) is obtained is added in rotary evaporator, and nanometer is obtained after rotary evaporation
Al/CuO-AP compound particles containing energy.
2. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
Cu (NO in the step (1)3)2It is 1 with NaOH mol ratios:2~1:3；DMAC and H2O in the mixed solvents DMAC and H2O volume
Than for 3:1~5:1.
3. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
Reaction temperature is 80 DEG C~110 DEG C in the step (1)；Reaction time is 1~10min.
4. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
The dosage of nanometer CuO is aqueous isopropanols of the 0.10g~0.15g/200~300ml containing PVP in the step (2)；Containing PVP's
PVP concentration is 0.05%~0.15% (W/V) in aqueous isopropanol；The nanometer CuO of the PVP modifications and mole of Al Nanoparticles
Than for 1.0~1.8:1.
5. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
The ultrasonic reaction time that the nanometer CuO of PVP modifications is prepared in the step (2) is 4~5h；It is described to prepare the super of nanometer Al/CuO
The phonoresponse time is 1~1.5h.
6. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
Nanometer Al/CuO quality is 0.25~4 times of AP mass in the step (3)；The organic solvent is ethanol or acetone.
7. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
The ultrasonic reaction time is 10~25min in the step (3).
8. the synthetic method of a kind of nanometer of Al/CuO-AP according to claim 1 compound particles containing energy, it is characterised in that
Rotating evaporation temperature is 10~30 DEG C in the step (4)；The rotary evaporator rotating speed is 100~140rpm；Rotary evaporation
Time is 10~25min.
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| CN107056562A (en) * | 2017-04-25 | 2017-08-18 | 中国工程物理研究院化工材料研究所 | A kind of aluminium base trielement composite material and preparation method thereof |
| CN107119301A (en) * | 2017-04-28 | 2017-09-01 | 重庆大学 | Al/CuO nanotube thermites and preparation method thereof |
| CN108179456A (en) * | 2017-12-01 | 2018-06-19 | 姜向军 | A kind of preparation method of nanometer of thermite film |
| CN109680309B (en) * | 2019-03-06 | 2020-10-09 | 重庆大学 | Super-hydrophobic porous Al/CuO nano-aluminum thermal energy-containing composite material |
| CN110105157A (en) * | 2019-06-19 | 2019-08-09 | 中国工程物理研究院化工材料研究所 | A kind of microcapsule-type thermite and preparation method thereof |
| CN114143962A (en) * | 2021-12-01 | 2022-03-04 | 重庆大学 | Al/CuO nano energetic product |
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