CN105665718A - Preparation method of nano aluminum/ammonium perchlorate (Al/AP) energy-containing composite particles - Google Patents
Preparation method of nano aluminum/ammonium perchlorate (Al/AP) energy-containing composite particles Download PDFInfo
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- CN105665718A CN105665718A CN201610071321.XA CN201610071321A CN105665718A CN 105665718 A CN105665718 A CN 105665718A CN 201610071321 A CN201610071321 A CN 201610071321A CN 105665718 A CN105665718 A CN 105665718A
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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
- 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
- B22F1/16—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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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 a preparation method of nano aluminum/ammonium perchlorate (Al/AP) energy-containing composite particles. The preparation method comprises the steps that firstly, AP is added into organic solvents to be subjected to ultrasonic dissolution, and an AP solution is obtained; then nano Al is dispersed into the AP solution in an ultrasonic mode, and the AP solution containing the nano Al is obtained; and finally, the AP solution containing the nano Al is added into a rotary evaporator to be subjected to a rotary evaporation reaction through a solvent evaporation method, the solvent is removed, and the nano Al/AP composite particles are obtained. According to the preparation method, the nano Al serves as crystal nucleus so that AP can grow on the surface of the nano Al, agglomeration of the nano Al is effectively prevented, the contact area between the nano Al and AP is increased, and the heat release performance is improved; meanwhile, accurate and quantitative preparation of all components in the composite particles can be achieved; and operation is convenient in the preparation process, the preparation process is simple and safe, the cost is low, the purity of a product is high, and the preparation method is suitable for large-scale production.
Description
Technical field
The preparation method that the present invention relates to a kind of Energetic Nanomaterials, is specifically related to a kind of nanometer of Al/AP preparation method containing energy compound particle.
Background technology
Energetic Nanomaterials, due to low initial reaction temperature, overactivity energy and high burn rate, receives more and more attention. General by metal/metal oxide and or nano-particle and the matrix of inorganic/organic energetic material component form. Metal powder, because having increase energy, improve quick-fried heat and capacity for work, improving the advantages such as ignition performance, is widely used in energetic material. And Al powder is because of the heat release of its excellence and low-temperature oxidation ability and the advantage such as abundant, less costly of drawing materials, play an important role in energetic material field. And the particle diameter of Al powder is more little, specific surface area is more big, and specific surface energy is more high, both macro and micro can show make new advances, excellent performance. But Al Nanoparticles is easily reunited in application process and owing to its specific surface energy is big, can consume more binding agent and carry out moistening, cause that its processing is more difficult.
Ammonium perchlorate (AP) owing to its oxygen content is high, without heavy metal ion, have high thermal stability and chemical stability, and low price, production technology are simple, can be completely converted into stable gaseous product after burning, always by extensive concern.
Ma Zhenye etc. (Ma Zhenye, Li Fengsheng, Chen Aisi, Song Hongchang. Push Technology, 2004,25:373-376.) select micron aluminium powder to be prepared for Al/ ammonium perchlorate compound particle by solvent-anti-solvent method, investigate its impact on the performance of propellant. Result shows compared with simple biased sample, and in compound particle, AP is had certain catalytic action by Al powder; Compared with adding pure Al powder, after Al/AP compound particle is added propellant, high-temperature sample decomposition peak's temperature drop is low, and thermal discharge is greatly improved, it was shown that can significantly improve the thermal decomposition performance of AP and propellant after Al powder and AP Combined Processing.
Slocik, J.M. (Slocik is waited, J.M., Crouse, C.A., Spowart, J.E., Naik, R.R.Nanoletters, 2013, 13:2535-2540.) adopt inside bioprotein cage AP being filled into after treatment, then protein cage/Al the particle of load AP it is prepared for the method for Al Nanoparticles compound, the preparation of the Al particle that multilamellar protein cage is modified is achieved by changing the charged character in protein cage surface, result shows, compared with the simple aggregate sample of Al powder and AP and pure Al powder, compound particle after compound demonstrates more excellent exothermicity and combustibility, but owing to adding the component-bioprotein of non-energetic material, other performance (such as the compatibility and mechanical property) of propellant can be produced potential impact.
In its component of the compound particle of existing bibliographical information, aluminium powder is micron aluminium powder or its complicated process of preparation, it is difficult to produces in a large number, there is not yet the report of high-purity nm Al/AP compound particle.
Summary of the invention
It is an object of the invention to make up the deficiencies in the prior art, it is provided that a kind of nanometer of Al/AP is containing can the preparation method of compound particle. The present invention adopts solvent evaporated method to prepare Al/AP containing energy compound particle, nanometer Al/AP that described preparation method prepares compound particle containing energy be the composite forming nucleocapsid structure so that AP is coated on nanometer aluminium powder surface, the wherein good dispersion of nanometer Al, Al Nanoparticles and AP contact area reach to maximize, exothermicity increases substantially, and good with the compatibility of other components of propellant, processability is also improved.
The purpose of the present invention is achieved through the following technical solutions:
A kind of nanometer of Al/AP, containing the preparation method of energy compound particle, comprises the following steps:
(1) preparation of AP solution:
Ammonium perchlorate joins organic solvent for ultrasonic dissolve, obtain AP solution;
(2) preparation of the AP solution containing nanometer Al:
In the AP solution prepare nanometer Al ultrasonic disperse to step (1), obtain the AP solution containing nanometer Al;
(3) preparation of nanometer Al/AP compound particle:
The AP solution containing nanometer Al step (2) obtained joins rotary evaporation in rotary evaporator, obtains a nanometer Al/AP compound particle.
The particle diameter of described nanometer of Al is 10～200 nanometers.
The solution temperature of described step (1) ammonium perchlorate is preferably 15～25 DEG C.
In described step (1), organic solvent is preferably ethanol or acetone.
In described step (2) consumption is AP mass 0.25～4 times of nanometer Al.
In described step (2), the ultrasonic disperse time is preferably 10～15min.
In described step (3), solvent evaporating temperature is preferably 10～30 DEG C.
In described step (3), the rotating speed of rotary evaporator is preferably 100～140rpm.
In described step (3), solvent evaporation time is preferably 10～25min.
Its principle of solvent evaporated method is to utilize the dissolubility causing solute in solution due to the volatilization of solution in heating process to become very little, and then reaches supersaturation, and the precipitation again from solution. When solvent evaporated method is used for preparing composite, preparation process is easy to operate, simple and safe, and cost is low, and product purity is high, it is possible to achieve the preparation of each component accurate quantitative analysis in compound particle, can largely overcome problems of the prior art.
Beneficial effects of the present invention:
Nanometer Al/AP of the present invention is containing the preparation method of energy compound particle, select AP that Al Nanoparticles original position is made directly compound, nanometer Al as nucleus for AP in its superficial growth, effectively prevent the reunion of Al Nanoparticles, improve the dispersibility of nanometer Al, the existence of AP simultaneously can promote the oxidizing fire of nanometer Al. The preparation process of compound particle is easy to operate, and preparation technology simplifies, and is suitable to large-scale production, and the method extends to other containing preparing by compound particle. The present invention specifically includes advantages below:
1) nanometer Al/AP of the present invention is containing energy one layer of AP of compound particle Surface coating, can significantly improve a nanometer agglomeration traits for Al particle, improves the dispersibility of nanometer Al; Simultaneously because AP is coated on a nanometer Al surface so that the two contact area reaches to maximize, be conducive to improving exothermicity, it is also possible to improve its reciprocity in propelling and processability.
2) solvent evaporated method is adopted to prepare compound particle, preparation process is easy to operate, simple and safe, cost is low, and the volatilization of the only solvent owing to existing in preparation process, do not have influence on the changes of contents of each component in compound particle so that each constituent content of compound particle keeps constant in preparation process, and in preparation process and be not introduced into other impurity, product purity is high.
3) present invention is based on solvent evaporated method, by Al Nanoparticles and AP direct combination, prepares nanometer Al/AP composite material containing energy, and this method is applicable to prepare highly purified composite in a large number.
Describe the present invention below in conjunction with specific embodiment. Protection scope of the present invention is not limited with detailed description of the invention, but is defined in the claims.
Accompanying drawing explanation
The Al/AP of Fig. 1 embodiment 1 preparation XRD figure containing energy compound particle.
The Al/AP of Fig. 2 embodiment 1 preparation SEM figure containing energy compound particle.
Detailed description of the invention
Embodiment 1
A kind of nanometer of Al/AP, containing the preparation method of energy compound particle, comprises the following steps:
(1) preparation of AP solution: under 15 DEG C of conditions, joins ultrasonic dissolution in 50ml acetone by 0.45g raw material A P, obtains the solution containing AP.
(2) preparation of the AP solution containing nanometer Al: under 15 DEG C of conditions, in the AP solution prepare 0.30g nanometer of Al ultrasonic disperse to step (1), after ultrasonic 10min, obtains the AP solution containing nanometer Al.
(3) preparation of nanometer Al/AP compound particle: adopt solvent evaporated method, the AP solution containing nanometer Al step (2) obtained joins in rotary evaporator, control rotary evaporator reaction temperature be 15 DEG C, rotating speed be 140rpm, after question response carries out 15min, wall obtains a nanometer Al/AP compound particle.
XRD, FESEM are as depicted in figs. 1 and 2. Result shows that particle diameter is 50-100nm containing energy compound particle particle spherical in shape. Embodiment 2
A kind of nanometer of Al/AP, containing the preparation method of energy compound particle, comprises the following steps:
(1) preparation of AP solution: under 20 DEG C of conditions, joins ultrasonic dissolution in 60ml ethanol by 0.15g raw material A P, obtains the solution containing AP.
(2) preparation of the AP solution containing nanometer Al: under 20 DEG C of conditions, in the AP solution prepare 0.225g nanometer of Al ultrasonic disperse to step (1), after ultrasonic 15min, obtains the AP solution containing nanometer Al.
(3) preparation of nanometer Al/AP compound particle: adopt solvent evaporated method, the AP solution containing nanometer Al step (2) obtained joins in rotary evaporator, control rotary evaporator reaction temperature be 10 DEG C, rotating speed be 100rpm, after question response carries out 20min, wall obtains a nanometer Al/AP compound particle.
Embodiment 3
A kind of nanometer of Al/AP, containing the preparation method of energy compound particle, comprises the following steps:
(1) preparation of AP solution: under 25 DEG C of conditions, joins ultrasonic dissolution in 50ml ethanol by 0.45g raw material A P, obtains the solution containing AP.
(2) preparation of the AP solution containing nanometer Al: under 25 DEG C of conditions, in the AP solution prepare 0.113g nanometer of Al ultrasonic disperse to step (1), after ultrasonic 15min, obtains the AP solution containing nanometer Al.
(3) preparation of nanometer Al/AP compound particle: adopt solvent evaporated method, the AP solution containing nanometer Al step (2) obtained joins in rotary evaporator, control rotary evaporator reaction temperature be 30 DEG C, rotating speed be 120rpm, after question response carries out 25min, wall obtains a nanometer Al/AP compound particle.
Through characterizing, nanometer Al/AP of embodiment 2 and embodiment 3 preparation is containing energy compound particle, its XRD, FESEM and Fig. 1 and Fig. 2 basic simlarity.
Claims (7)
1. nanometer Al/AP is containing a preparation method for energy compound particle, comprises the following steps:
(1) preparation of AP solution:
Ammonium perchlorate joins organic solvent for ultrasonic dissolve, obtain AP solution;
(2) preparation of the AP solution containing nanometer Al:
In the AP solution prepare nanometer Al ultrasonic disperse to step (1), obtain the AP solution containing nanometer Al;
(3) preparation of nanometer Al/AP compound particle:
The AP solution containing nanometer Al step (2) obtained joins rotary evaporation reaction in rotary evaporator, obtains a nanometer Al/AP compound particle.
2. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: the particle diameter of described nanometer of Al is 10～200 nanometers.
3. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: in described step (1), the solution temperature of ammonium perchlorate is 15～25 DEG C.
4. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: in described step (1), organic solvent is ethanol or acetone.
5. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: in described step (2) 0.25～4 times of the quality that consumption is AP of nanometer Al.
6. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: in described step (2), the ultrasonic disperse time is 10～15min.
7. according to claim 1 nanometer Al/AP containing can the preparation method of compound particle, it is characterised in that: in described step (3), solvent evaporating temperature is 10～30 DEG C; The rotating speed of rotary evaporator is 100～140rpm; Solvent evaporation time is 10～25min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282919A (en) * | 2017-06-14 | 2017-10-24 | 南京师范大学 | A kind of nanometer aluminium powder/paraffin compound particle containing energy and its preparation method and application |
| CN115947640A (en) * | 2023-01-31 | 2023-04-11 | 南京师范大学 | Aluminum powder/fluoropolymer/ammonium perchlorate energetic composite particle and preparation method thereof |
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| US3953256A (en) * | 1973-08-22 | 1976-04-27 | Thiokol Corporation | Propellants and pyrotechnic compositions containing aluminum-coated ammonium perchlorate |
| US4115166A (en) * | 1970-01-12 | 1978-09-19 | Aerojet-General Corporation | Coated ammonium perchlorate |
| US20050072501A1 (en) * | 2001-01-12 | 2005-04-07 | Blau Reed J. | Moisture-resistant black powder substitute compositions and method for making same |
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| CN103044175A (en) * | 2012-12-05 | 2013-04-17 | 浙江大学 | High-efficient coating method of boron particles |
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| US3953256A (en) * | 1973-08-22 | 1976-04-27 | Thiokol Corporation | Propellants and pyrotechnic compositions containing aluminum-coated ammonium perchlorate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282919A (en) * | 2017-06-14 | 2017-10-24 | 南京师范大学 | A kind of nanometer aluminium powder/paraffin compound particle containing energy and its preparation method and application |
| CN115947640A (en) * | 2023-01-31 | 2023-04-11 | 南京师范大学 | Aluminum powder/fluoropolymer/ammonium perchlorate energetic composite particle and preparation method thereof |
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