CN102441668B - Method for preparing Fe/Al micro-nano composite powder - Google Patents
Method for preparing Fe/Al micro-nano composite powder Download PDFInfo
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- CN102441668B CN102441668B CN 201110353225 CN201110353225A CN102441668B CN 102441668 B CN102441668 B CN 102441668B CN 201110353225 CN201110353225 CN 201110353225 CN 201110353225 A CN201110353225 A CN 201110353225A CN 102441668 B CN102441668 B CN 102441668B
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Abstract
The invention discloses a method for preparing Fe/Al micro-nano composite powder. The method comprises the following steps of: scattering Al powder in kerosene by using ultrasonic oscillation; stirring to form a uniform mixed solution; injecting Fe(CO)5 at 180-300 DEG C and evenly mixing Al powder and Fe(CO)5 in the kerosene; heating to basically finish a coating reaction, wherein the temperature is always kept at 180-300 DEG C in the whole process; centrifugally pumping out reaction products; repeatedly washing the products with absolute ethyl alcohol; and after the product is cleaned, drying in vacuum to obtain Fe/Al composite powder. The method has simple technology and low cost; the synthesized Fe/Al micro-nano composite powder is a nuclear shell structure comprising micro-nano Al coated with nano-Fe, and has good dispersity and excellent thermal property; moreover, the Fe/Al micro-nano composite powder has an obviously higher activity in reaction with O2 in comparison with the raw material Al powder; and the heat output is remarkably increased, the heat release is quicker and more intensive, and the burning process is greatly improved.
Description
Technical field
The present invention relates to the manufacture method of Micron-nano composites, the Fe/Al composite granule for preparing with the method is a kind of nucleocapsid structure that is comprised of nanometer Fe coating micron Al, and has very high fuel factor.
Background technology
The Al powder has the very high combustion heat and volume calorific value as a kind of good fuel agent, is widely used in the manufacturing of multiple energetic material, such as solid rocket propellant, high explosive and pyrotechnics, Loading Materials for Initiating Explosive Devices etc.But the micron aluminium powder is owing to exist combustion powered slow, the problem such as firing delay long, burning is insufficient, and its potential high heating value can't be fully used; On the other hand, aluminium has very strong affinity to oxygen, and particularly for micron-sized active metal Al, its specific area is very large, is exposed to outer as easy as rolling off a log the combination with oxygen of surface atom and oxidized, the oxide-film (Al of formation one deck densification
2O
3), thereby aluminium powder is lost activity, these have all limited the application of micron aluminium powder to a great extent.
In recent years, the study on the modification of the preparation of Micron-nano composites and micron metal powder has caused the generally attention of material supply section educational circles.Wherein, it is very fast that particle surface coats the modification technology development, becomes the research focus of new material surface and interface scientific domain.Studies show that it is to promote the Al particle to light a fire, improve efficiency of combustion, effective method that micron order Al powder is carried out surface coating processing.The researcher has adopted many kinds of substance that the micron aluminium powder is coated modification, such as aspect the organic matter, and C
13F
27COOH, NC etc.; The metal oxide aspect, Al
2O
3Connection metal, Ni, Ag, Cu, Fe etc.Adopt nano-iron particle to coat a micron aluminium powder, can prevent the problem that reoxidizes on Al powder surface on the one hand, the thermal response that improves micron Al powder is active; On the other hand, the iron oxide (Fe of the oxidized generation of Nanoscale Iron simple substance
2O
3), the combustion catalyst for commonly used has the effect of good catalytic action and combustion stability.The mixture of itself and Al powder consists of the main body of thermite, after the initiation that is subject to heat or mechanical force, violent redox reaction can occur, and emit a large amount of heat, has high exothermal nature.Preparation Fe/Al composite material of core-shell structure becomes one of the most popular research method of present coating Al, also is to seek the developing direction that the fuel factor of Al further takes full advantage of.
At present, the preparation method of metal particle coating micron aluminium powder mainly contains galvanoplastic and electroless plating method.The comparison in equipment of galvanoplastic is complicated, and cost is higher.Electroless plating method technique is simpler, and cost is lower.Yet Al belongs to amphoteric metal, and is all unstable in acidity or alkali plating solution, and is easy to cause the decomposition of plating bath, improved to a great extent the difficulty of preparation process.Liquid-phase chemistry deposition technique is the important method of preparation composite, and this method relatively is easy to form nucleocapsid structure, and it is controlled to coat thickness, and technology and equipment is simple, and is with low cost.Report that at present the method for utilizing the precursor decomposition to deposit to Al powder surface is very few, the present invention intends adopting liquid-phase chemistry deposition technique, and the preparation clad is even, fine and close Fe/Al composite material of core-shell structure.
Summary of the invention
The object of the present invention is to provide the method for the micro-nano composite granule of a kind of Fe/Al of preparation, the method technique is simple, with low cost, the micro-nano composite granule of the Fe/Al that synthesizes is a kind of nucleocapsid structure that is comprised of nanometer Fe coating micron Al, and have good dispersiveness and excellent hot property, itself and O
2The activity of reaction is apparently higher than raw material A l powder, and thermal discharge is greatly improved, and thermal release is quicker, more concentrated, and combustion process is significantly improved.
The invention provides the preparation method of the micro-nano composite granule of a kind of Fe/Al, it is characterized in that: the method comprises the steps:
(1) the Al powder is scattered in the kerosene, and uses sonic oscillation so that it is dispersed in the kerosene, stirring makes it form uniform mixed solution, injects Fe (CO) at 180 ℃～300 ℃
5The time, make Al powder and Fe (CO)
5Mix in kerosene, heating is finished coating reaction substantially, and the temperature of this process remains at 180 ℃～300 ℃;
(2) reacted product is carried out centrifugal detaching, then with absolute ethyl alcohol product is carried out cyclic washing, dry in a vacuum after the washes clean, obtain the Fe/Al composite powder.
The present invention with adopt additive method to prepare the Fe/Al composite powder to compare and have the following advantages:
1) the present invention adopts liquid-phase chemistry deposition technique to prepare the Fe/Al composite construction, and technique is simple, and is with low cost.Compare with galvanoplastic, do not need complicated equipment, compare with electroless plating method, do not need harsh process conditions;
2) the source of iron Fe (CO) of the present invention's employing
5Just Fe can be all be decomposed at 180 ℃, the amount that is coated on the shell of Fe on the Al powder can be accurately controlled;
3) the micro-nano composite granule clad of Fe/Al of the present invention's preparation is even, complete, shows good hot property.Compare with raw material A l powder, at identical temperature section, itself and O
2The thermal discharge of reaction is greatly improved, and thermal release is quicker, and is more concentrated, and weightening finish is violent, and weightening finish speed is improved significantly.
Description of drawings
Fig. 1 is the used device schematic diagram of the present invention, wherein, and 1, argon bottle 2, oil bath pan 3, reactor 4, condenser pipe 5, thermometer 6, syringe 7, KMnO
4Solution 8, H
2O;
Fig. 2 is the SEM collection of illustrative plates of the micro-nano composite granule of Fe/Al of preparation, wherein, and (a), (b) be respectively low power and the high power SEM photo of original Al powder, (c), (d) be respectively low power and the high power SEM photo of Fe/Al composite powder;
Fig. 3 is the SEM collection of illustrative plates of the micro-nano composite granule cross section of Fe/Al of preparation, (a), (b) be respectively low power and the high power SEM photo of Fe/Al composite powder cross section, (c) is the SEM-EDX photo of Fe/Al composite powder cross section;
Fig. 4 is the XRD collection of illustrative plates of the micro-nano composite granule of Fe/Al of preparation;
Fig. 5 (a) is the TG curve of original Al powder and Fe/Al composite powder for the micro-nano composite granule fuel factor of Fe/Al (TG-DTA) curve of preparation, (b) is the DTA curve of original Al powder and Fe/Al composite powder.
The specific embodiment
The present invention uses carbonyl iron (Fe (CO)
5) as presoma, utilize it to decompose the characteristic that generates the iron particle at 180 ℃ and produce clad, Fe (CO)
5When decomposing generation iron, generate CO.CO is a kind of reducing gas, and this has further prevented oxidation so that our coating system is in the reducing atmosphere;
The Al powder is scattered in the kerosene, and use sonic oscillation so that it has dispersed preferably in kerosene, all adopt agitating device that solution is stirred in the whole experimentation, form uniform mixed solution by sonic oscillation with after stirring, inject Fe (CO) at 180 ℃
5The time, so that the three is in the more uniform state of mixing, continuous heating as far as possible, by the change color of observing response device the inside, when color becomes black, continuous heating a period of time again, guarantee that coating reaction finishes substantially, the temperature of this process remains at 180 ℃;
Reacted product is carried out centrifugal detaching, then with absolute ethyl alcohol product is carried out cyclic washing, dry in a vacuum after the washes clean, obtain the Fe/Al composite powder.
Embodiment 1
The present invention adopts kerosene to make reagent, under 180,240,300 ℃ of temperature, utilizes carbonyl iron to decompose generation iron particle and coats a micron aluminium, and in experiment, we have done the experiment of several groups of different Fe/Al mol ratios; Lower mask body is with under 180 ℃ of temperature, and the Fe/Al mol ratio is that 0.5: 1 coating is example, comes its process and covered effect are specified.
Experimental provision as shown in Figure 1; at first the micron aluminium powder is dispersed in the kerosene; insert reactor 3; and with sonic oscillation effect 10 minutes; aluminium powder is had in kerosene preferably disperse, reactor 3 connects respectively oil bath pan 2, thermometer 5, protective gas (high-purity argon gas 1) and condenser pipe 4, syringe 6.10min before heating, high-purity argon gas is passed in the reactor 3, to get rid of the oxygen in the reactor 3, then reactor 3 is heated, when thermometer 5 is shown as 180 ℃ of left and right sides, toward reactor 3 interior injection carbonyl irons, substantially finish in order to ensure coating reaction, be 60min the duration of heat that we select, and the temperature of this process remains at 180 ℃.The KMnO that the device rear portion connects
4Solution 7 and H
2O solution 8 is used for processing the pernicious gas that produces in the experimentation.Behind the heating 60min, stopped heating allows experimental system naturally cool off, and behind the cool to room temperature, will react afterwards that products therefrom carries out centrifugation, and with absolute ethyl alcohol powder be carried out cyclic washing, remains in organic solvent on the powder with removal.After 4-5 the washing, powder is carried out drying in a vacuum, namely obtain having the micro-nano composite granule of Fe/Al of complete nucleocapsid structure.
Figure 2 shows that the environmental scanning photo that makes composite particles, wherein, Fig. 2 a, Fig. 2 b are respectively the SEM photo of original Al powder under low power and high power visual field, and Fig. 2 c, Fig. 2 d are respectively the SEM photo of prepared Fe/Al composite powder under low power and high power visual field.From figure, can clearly observe, after the coating, micron Al particle surface obviously has one deck closely, continuous, uniform fine particle, although this granule has a small amount of reunion in the part, generally still uniformly, fine and close being distributed on micron surface of Al powder.
Figure 3 shows that the environmental scanning photo that makes the composite particles cross section, wherein, Fig. 3 a, Fig. 3 b are respectively the SEM photo of cross section under low power and high power visual field of obtained Fe/Al composite powder, and Fig. 3 c is the SEM-EDX photo of cross section under the high power visual field of obtained Fe/Al composite powder.By Fig. 3, can intuitively clearly observe Al nuclear surface and really coated by material intact, that be different from nucleome.By the EDX line scanning, can determine that outer material is Fe, inner core materials is Al.
Composite particles is carried out the X-rays diffraction detect, the result as shown in Figure 4.Fig. 4 shows that prepared micro-nano composite granule only has the diffraction maximum of Fe, Al phase, is pure Fe/Al composite granule.
Figure 5 shows that original Al powder and differential thermal-thermogravimetric (TG-DTA) curve map that makes the Fe/Al composite powder.Wherein, (a) the TG curve of original Al powder and Fe/Al composite powder (heated perimeter: 20-1400 ℃, firing rate: 20 ℃/min, heating atmosphere: O
2), (b) the DTA curve of original Al powder and Fe/Al composite powder (heated perimeter: 20-1400 ℃, firing rate: 20 ℃/min, heating atmosphere: O
2).Can be as drawing a conclusion by Fig. 5: after coating Fe, Fe/Al-O
2The exothermic heat of reaction stage than Al-O
2Obviously in advance; In same temperature ranges stated, Fe/Al-O
2Thermal discharge than Al-O before coating
2Thermal discharge just be greatly improved; Al powder and O after the coating
2Reaction rate improves greatly, and thermal release is quicker, and is more concentrated; Fe/Al-O
2Weight gain obviously be much higher than coating before, it is more violent to increase weight, rate of body weight gain obviously improves.
Other examples of implementation mainly are the different of the temperature that coats and Fe/Al mol ratio, by changing the mol ratio of temperature of plate and Fe/Al, can obtain covered effect under the mol ratio of three kinds of different temperature of plate and Fe/Al and the thickness of clad; It is as shown in the table to test resulting result, in table, we can see, embodiment 2,3 is respectively under 240,300 ℃ of temperature, the mol ratio of Fe/Al is the coating experiment of carrying out in 0.3: 1 and 0.7: 1 time, other operation and embodiment 1 in the experimentation are identical, their prepared composite particles are analyzed, result and embodiment 1 are basic identical, nanometer Fe uniform particles, fine and close being coated on the Al particle, and the thermal discharge of composite particles is greatly improved before the coating with weightening finish.
| Temperature | The Fe/Al mol ratio | Coating thickness | Covered effect | |
| Embodiment 1 | 180℃ | 0.5∶1 | 1080nm | Evenly, fine and |
| Embodiment | ||||
| 2 | 240℃ | 0.3∶1 | 950nm | Evenly, the fine and close coating |
| Embodiment 3 | 300℃ | 0.7∶1 | 1140nm | Evenly, the fine and close coating |
Usually, the Fe/Al mol ratio is between 0.3: 1 to 0.7: 1, and heating-up temperature is between 180 ℃ to 300 ℃, and drying can be carried out at room temperature or in the vacuum environment of heat (not being higher than 100 ℃).
The present invention not only is confined to the above-mentioned specific embodiment; persons skilled in the art are according to content disclosed by the invention; can adopt other multiple specific embodiment to implement the present invention; therefore; every employing project organization of the present invention and thinking; do some simple designs that change or change, all fall into the scope of protection of the invention.
Claims (1)
1. method for preparing the micro-nano composite granule of Fe/Al is characterized in that:
(1) micron Al powder is scattered in the kerosene, and uses sonic oscillation so that it is dispersed in the kerosene, stirring makes it form uniform mixed solution, injects Fe (CO) at 180 ℃～300 ℃
5The time, make Al powder and Fe (CO)
5Mix in kerosene, wherein the Fe/Al mol ratio is between 0.3:1 to 0.7:1, and heating is finished coating reaction substantially, and the temperature of this process remains at 180 ℃～300 ℃; Fe (CO)
5When decomposing generation iron particle, generate CO, so that the coating system is in the reducing atmosphere, further prevent oxidation;
(2) reacted product is carried out centrifugal detaching, then with absolute ethyl alcohol product is carried out cyclic washing, dry in the washes clean final vacuum, obtain the micro-nano composite granule of Fe/Al.
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| CN103060770B (en) * | 2012-12-04 | 2014-12-17 | 华中科技大学 | Preparation method of iron-clad aluminum type composite powder and product thereof |
| CN104551005B (en) * | 2015-01-07 | 2017-01-04 | 北京化工大学 | A kind of nanoscale nucleocapsid structure thermite and preparation method thereof |
| CN107162406B (en) * | 2017-06-15 | 2018-02-23 | 南京安达玻璃技术有限公司 | A kind of high printing opacity heat-insulating and energy-saving float glass composition |
| CN108655414A (en) * | 2018-06-11 | 2018-10-16 | 合肥学院 | A kind of quick magnanimity prepares the simple and easy method of two dimension Ag micro Nano materials |
| CN110197752B (en) * | 2019-06-13 | 2021-07-27 | 深圳市麦捷微电子科技股份有限公司 | Insulating powder process for hard-to-passivate magnetic powder and magnetic powder prepared by using insulating powder process |
| CN113817977A (en) * | 2021-09-23 | 2021-12-21 | 南京金鲤新材料有限公司 | Preparation method of plasma spraying Al-Fe intermetallic compound powder |
| CN114309593B (en) * | 2021-09-24 | 2024-04-05 | 中北大学 | Preparation method of multielement transition metal coated micron aluminum composite fuel |
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