CN101921160A - Preparation method of super-thermite Al/PbO nano-composite energetic material - Google Patents
Preparation method of super-thermite Al/PbO nano-composite energetic material Download PDFInfo
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Abstract
The invention discloses a super-thermite Al/PbO nano-composite energetic material and a preparation method thereof. The super-thermite Al/PbO nano-composite energetic material consists of nano-grade aluminum powder and PbO, wherein the molar ratio of aluminum powder to PbO is (1:3)-(1:1), the grain diameter of aluminum powder is 20-100nm, and the grain diameter of obtained nano-composite energetic material is 50nm-150nm. The method comprises the following steps: respectively dissolving organic or inorganic lead salt and organic or inorganic base in alcoholic solution; dissolving completely, mixing the alcoholic solution of the lead salt and the base to generate lacte sol; and finally adding nano aluminum powder, completely mixing, filtering, washing and drying. The method has simple process, convenient operation and high safety performance and is easy to control, and the obtained nano-composite energetic material Al/PbO has excellent catalytic effect on the combustion of a double-base solid propellant when being taken as a combustion catalyst, thus significantly improving the burning speed of the propellant and reducing the pressure exponent.
Description
Technical field
The present invention relates to a kind of super thermite Al/PbO Nanocomposite Energetic Materials and preparation method thereof, belong to the nano material preparation technical field, this Nanocomposite Energetic Materials can be used as the combustioncatalysts that double-basis is a propelling agent.
Background technology
Double-basis is that propelling agent is a class high energy fuels that is used for rocket and guided missile, but its shortcoming is that combustion speed is lower, pressure index is higher, needs to add combustioncatalysts and regulates combustionproperty.Discover that double-basis is that an amount of plumbous catalyzer of adding not only can improve combustion speed in the propelling agent, can also realize " platform " or " wheat is spread " aptitude to burn.Yet, continuous development improvement along with the rocket-powered missile technology, it is to propulsion source---and the requirement of propelling agent is also more and more higher, thus need the efficient burning catalyzer of development of new to satisfy the needs of novel solid propelling agent development, thus be implemented in the ultimate aim of using on the high-performance weapon.In addition, double-basis is the propulsion source of propelling agent as rocket and guided missile, and it must pursue very high energy.Though yet the use of inert catalyst has improved the combustionproperty of propelling agent, also reduced its energy simultaneously.Therefore, explore and exploitation contain can burningrate catalyst just become a important directions in the research of novel solid propelling agent.Contain can catalyzer important feature be exactly itself contain can, it is both can be collaborative improving combustionproperty with other component in the propellant formulation in double-basis, but also can discharge self-energy to guarantee even to improve the energy characteristics of propelling agent.
Nanometer aluminium powder is applied in the solid propellant as high energy fuels, has been proved to be able to improve widely propellant burning property.Because its high rate of heat release can improve the heat release rate in the condensed phase, has higher heat flux so contain the propelling agent of nanometer aluminium powder, thereby can improve combustion speed.Foreign study is the result show, compares with common aluminium powder, and nanometer aluminium powder has the lower bound temperature of lower beginning chemical reaction, and has bigger specific surface area and reduced size, so it can significantly promote solid propellant combustion rate and reduce burning rate pressure exponent.Yet nanometer aluminium powder is because greatly specific surface area, very high specific surface energy and specific surface activity, its reunite easily and the surface very easily oxidized and lose activity; In addition, the non-compatibility of nanometer aluminium powder and organic solvent and corroding easily in air, acid, alkaline medium makes its application in solid propellant be subjected to considerable restraint.
The reactive systems of the nano level metal/non-metal base energetic material that obtains through Combined Processing by two components, be called super thermite (Super Thermites) or the intermolecular mixture of metastable state (Metastable Intermolecular Composites, MIC), it generally is the mixture that the stronger metal/non-metal oxide compound of nano level aluminium powder and oxidisability is formed, it has following benefit as combustioncatalysts: first, weaken even eliminate the agglomeration that nanometer aluminium powder causes because of self motive power, improve the dispersiveness of nanometer aluminium powder effectively, thereby can guarantee giving full play to of its excellent nano functional characteristic; The second, performance nano metal/nonmetal oxide is applied to the excellent properties that solid propellant brings, and not only can improve propellant burning rate, can also reduce pressure index; The 3rd; choose nano metal/nonmetal oxide and nanometer aluminium powder Combined Processing; in the protection active while of nanometer aluminium powder; can make full use of the synergistic effect of two kinds of material functions; the excellent functional performance of nanoparticle is improved greatly, give full play to its effect as the SOLID PROPELLANT COMBUSTION catalyzer.
The preparation method of MIC mainly contains mechanical-physical composite algorithm (Sanders V E at present, Asay B W, Foley T J, et al.Journal of Propulsion and Power. (2007) 707-714), this method is easy but it is difficult to make superfine powder closely to mix, and there is the inhomogeneous and skewness of grain-size in the sample of preparation, easily introduces some impurity and makes and polluted the not high shortcoming of purity between particle surface and the interface; Sol-gel chemical method (Tillotson T M, Gash A E, Simpson R L, et al.Journal of Non-Crystalline Solids. (2001) 338-345), by this legal system be equipped with sample purity and uniformly dispersed better, but it is worthless in some applications that the porousness of resulting composite makes it, but the restriction that used by the gel-type material, simultaneously since in the solution of stirring need with a very definite gel generation introduce period nanometer aluminium powder make its difficulty boost productivity, in addition, preparation technology is loaded down with trivial details for this method, preparation cycle is long, needs high-tension apparatus when adopting supercritical drying, and cost is higher; Reaction suppresses grinding technique (Dreizin E L, Schoenitz M.US Patent Application 20060053970.2006), flexible and the highly versatile of this technology, the limitation of its maximum is that the oneself that machinery triggers keeps before the reaction, select to interrupt the bad control of time point of process of lapping, the product dispersed uniform is bad, and the security of ball mill operation when adopting this legal system to be equipped with remains to be investigated.
In sum, new low cost, high security and the synthetic easy super thermite of exploitation has important practical significance as the novel energy combustioncatalysts of using in the solid propellant that contains.
Summary of the invention
The double-basis that can be used as that the purpose of this invention is to provide that a kind of safety performance height, product are uniformly dispersed, preparation cycle is short and production cost is low is that containing of propelling agent can combustioncatalysts---super thermite Al/PbO Nanocomposite Energetic Materials overcomes disadvantages of background technology.
Another object of the present invention is to provide the preparation method of above-mentioned super thermite Al/PbO Nanocomposite Energetic Materials.
The object of the present invention is achieved like this:
A kind of super thermite Al/PbO Nanocomposite Energetic Materials, its nano level aluminium powder and PbO mol ratio are: (1: 3)～(1: 1), described aluminium powder particle diameter is 20～100nm, the particle diameter of the Nanocomposite Energetic Materials that obtains is 50nm～150nm.
The preparation method of above-mentioned super thermite Al/PbO Nanocomposite Energetic Materials comprises the steps:
(1) with the organic or inorganic lead salt, organic or inorganic alkali is dissolved in the alcoholic solution respectively;
(2) fully after the dissolving, the two alcoholic solution is mixed, generate oyster white colloidal sol;
(3) add nanometer aluminium powder, fully stir, filter, washing, dry getting final product.
Described organic or inorganic lead salt is plumbic acetate, lead nitrate or lead citrate, and pre-treatment was carried out in oven dry in advance before the organic or inorganic lead salt used, and removed its contained crystal water.
Described organic or inorganic alkali is NaOH, KOH, LiOH, sodium ethylate, potassium ethylate, triethylamine or quadrol.
Described alcoholic solution is ethylene glycol, glycerol, methyl alcohol, ethanol or propyl alcohol, and most preferred alcoholic solution is an ethylene glycol.
Advantage of the present invention and positively effect: (1) is raw material with organic or inorganic lead salt, inorganic or organic bases, cheap and easy acquisition; (2) technology is simple, and is easy to operate, is easy to control, the safety performance height; (3) be reflected at liquid-phase mixing under the ultrasound condition, nanometer aluminium powder and Pb (OH)
2The colloidal sol dispersive is better, and the product that finally obtains is uniformly dispersed; (4) preparation cycle is short; (5) cut down the consumption of energy, production cost is low.Nanocomposite Energetic Materials Al/PbO of the present invention is that the burning of solid propellant has good catalytic effect as combustioncatalysts to double-basis, can significantly improve propellant burning rate and reduce pressure index.
Description of drawings
Fig. 1 is the SEM photo of the product for preparing of the embodiment of the invention 1 and 2;
Fig. 2 is the XRD spectra of the product for preparing of the embodiment of the invention 1;
Fig. 3 is the XRD spectra of the product for preparing of the embodiment of the invention 2;
Fig. 4 is the burningrate curve behind the super thermite of interpolation the present invention in double-base propellent.
Embodiment
Select the organic or inorganic lead salt for use, organic or inorganic alkali is raw material, with pretreated organic or inorganic lead salt, organic or inorganic alkali respectively in ultrasound condition lower magnetic force (machinery) stirring and dissolving in ethylene glycol solution, after treating to dissolve fully that the two is miscible, generate oyster white Pb (OH) at once
2Colloidal sol adds nanometer aluminium powder subsequently, uses magneton agitator stirred for several hour (2-6h) under the water bath with thermostatic control condition, after reaction soln separates, with deionized water and absolute ethanol washing precipitation several, after drying is handled a few hours in vacuum drying oven again, make product.
Concrete preparation method comprises the steps:
(1) select the organic or inorganic lead salt for use, organic or inorganic alkali is raw material; The preferred plumbic acetate of described lead salt; Described alkali is preferably sodium hydroxide or potassium hydroxide.
(2) with pretreated organic lead-salt (drying dewaters) and mineral alkali respectively in ultrasound condition lower magnetic force (machinery) stirring and dissolving in ethylene glycol solution, after treating to dissolve fully that the two is miscible, generate oyster white Pb (OH) at once
2Glue adds nanometer aluminium powder after a moment.
Pretreated lead salt concentration is 0.08～0.8mol/L, adds alkali 0.08～1.2mol in every liter of lead salt solution, and wherein alkali concn is 0.08～0.8mol/L.
(3) use magneton agitator stirred for several hour (2-6h) under the water bath with thermostatic control condition, after reaction soln separates, with deionized water and absolute ethanol washing precipitation several;
(4) after drying is handled a few hours in vacuum drying oven again, make product.
Aforesaid operation, water bath with thermostatic control condition are 60～120 ℃, and the vacuum drying oven temperature is 60～110 ℃, and drying time is 20～30h.
Embodiment 1:
Accurately weighing 1.3g (4mmol) is through pretreated lead acetate and 0.352g (8.8mmol) sodium hydroxide, under the room temperature in the ultrasonic respectively ethylene glycol that is dissolved in 10ml and 22ml, after treating to dissolve fully that the two is miscible, at once obtain oyster white colloidal sol, add 0.1008g (3.7mmol) nanometer aluminium powder (about 50nm) after 4～6 minutes, water bath with thermostatic control (80 ℃) lower magnetic force agitator stirs (Mot=3) 2.5h.After reaction soln separates, precipitate with deionized water and absolute ethanol washing several, and after in vacuum drying oven, handling 28h, promptly get the super thermite of black powder shape Al/PbO.
With field emission scanning electron microscope (SEM), X-ray powder diffraction (XRD), infrared spectrometer (IR), x-ray fluorescence spectrometry (XRF) and thermogravimetric analyzer (TG) product being carried out structure properties characterizes.
Shown in Figure 1A, product is equally distributed spherical Al/PbO nanocrystal, and particle diameter is between 50～150nm.
As shown in Figure 2, the standard diagram card of Al and PbO matches among the spacing d value of product feature diffraction peak and the standard JCPDS, exists the characteristic diffraction peak of these two kinds of materials and peak shape good.
Embodiment 2
Accurately weighing 1.3g (4mmol) is through three pretreated hydration lead acetate and 0.493g (8.8mmol) potassium hydroxide, under the room temperature in the ultrasonic respectively ethylene glycol that is dissolved in 10ml and 22ml, after treating to dissolve fully that the two is miscible, at once obtain oyster white colloidal sol, add 0.1008g (3.7mmol) nanometer aluminium powder (about 50nm) after 4～6 minutes, water bath with thermostatic control (75 ℃) lower magnetic force agitator stirs (Mot=3) 2.0h.After reaction soln separates, precipitate with deionized water and absolute ethanol washing several, and after in vacuum drying oven, handling 24h, promptly get the super thermite of black powder shape Al/PbO.
With field emission scanning electron microscope (SEM), X-ray powder diffraction (XRD), infrared spectrometer (IR), x-ray fluorescence spectrometry (XRF) and thermogravimetric analyzer (TG) product being carried out structure properties characterizes.
Shown in Figure 1B, product is equally distributed spherical Al/PbO nanocrystal, and particle diameter is between 50～150nm.
As shown in Figure 3, the standard diagram card of Al and PbO matches among the spacing d value of product feature diffraction peak and the standard JCPDS, exists the characteristic diffraction peak of these two kinds of materials and peak shape good.
Embodiment 3
Similar to Example 1, different is the organic bases triethylamine of selecting 8.8mmol for use, has prepared the spherical Al/PbO nanocrystal of particle diameter between 50～150nm in ethanolic soln equally.
The contrast experiment finds, makes spent glycol as solvent, the product good dispersion degree for preparing, and particle diameter is more even.
Embodiment 4
The basic components of the double-base propellent that the katalysis performance test of super thermite Al/PbO Nanocomposite Energetic Materials is adopted is: nitro-cotton (NC, 12.0%N) 59%, nitroglycerine (NG) 30%, 8.5%, No. two centralite (C of diethyl phthalate (DEP)
2) 2.0%, other auxiliary agent 0.5%.Spice is pressed the 500g batching, and catalyzer is outer dosage, and add-on is 2.5%; The blank propelling agent sample of control group does not contain catalyzer.
Propelling agent by sample absorption-expelling water-put ripe-the conventional solvent-free companding shaping technology of rolling-being cut into medicinal strip makes.The combustion speed of sample adopts the target collimation method to record.The little powder column of the Φ 5 * 150mm side of having handled is coated 6 times with the polyvinyl alcohol solution dipping and dry, fire and fire the speed test in the fast instrument filling nitrogen slow-action formula then.Test temperature is 20 ℃, pressure range 2MPa～20MPa.
As can be seen from Figure 4, the super thermite Al/PbO Nanocomposite Energetic Materials that the embodiment 1 of adding 2.5% prepares makes double-base propellent significant raising occur, " platform " combustion zone occurs in 4MPa～14MPa pressure range in 2MPa～20MPa combustion speed.This catalyzer is at the catalytic efficiency Z of 2MPa～20MPa (Z=r
c/ r
0, r
0Be the combustion speed of blank formula, r
cFor containing the propellant burning rate of catalyzer) be respectively 2.54,2.12,1.77,1.59,1.43,1.33,1.30,1.35,1.33,1.35.At 8MPa～14MPa, the pressure index n of propelling agent is 0.37.
As seen, this catalyzer has shown significant combustion catalysis and good reduction pressure exponential ability, illustrates that this Nanocomposite Energetic Materials is a kind of combustioncatalysts efficiently.
Claims (10)
1. super thermite Al/PbO Nanocomposite Energetic Materials is characterized in that:
Nano level aluminium powder and PbO mol ratio are: (1: 3)～(1: 1).
2. super thermite Al/PbO Nanocomposite Energetic Materials according to claim 1, it is characterized in that: described aluminium powder particle diameter is 20～100nm.
3. super thermite Al/PbO Nanocomposite Energetic Materials according to claim 1, it is characterized in that: the particle diameter of Nanocomposite Energetic Materials is 50nm～150nm.
4. the preparation method of the described super thermite Al/PbO Nanocomposite Energetic Materials of claim 1 comprises the steps:
(1) with the organic or inorganic lead salt, organic or inorganic alkali is dissolved in the alcoholic solution respectively;
(2) fully after the dissolving, the two alcoholic solution is mixed, generate oyster white colloidal sol;
(3) add nanometer aluminium powder, fully stir, filter, washing, dry getting final product.
5. the preparation method of super thermite Al/PbO Nanocomposite Energetic Materials according to claim 4 is characterized in that: described organic or inorganic lead salt is plumbic acetate, lead nitrate or lead citrate.
6. the preparation method of super thermite Al/PbO Nanocomposite Energetic Materials according to claim 4 is characterized in that: described organic or inorganic alkali is NaOH, KOH, LiOH, sodium ethylate, potassium ethylate, triethylamine or quadrol.
7. the preparation method of super thermite Al/PbO Nanocomposite Energetic Materials according to claim 4 is characterized in that: described alcoholic solution is ethylene glycol, glycerol, methyl alcohol, ethanol or propyl alcohol.
8. the preparation method of super thermite Al/PbO Nanocomposite Energetic Materials according to claim 7 is characterized in that: described alcoholic solution is an ethylene glycol.
9. the preparation method of super thermite Al/PbO Nanocomposite Energetic Materials according to claim 4 is characterized in that: pre-treatment was carried out in oven dry in advance before described organic or inorganic lead salt used, and removed its contained crystal water.
10. one of any described super thermite Al/PbO Nanocomposite Energetic Materials of claim 1 to 3 can be used as the combustioncatalysts that double-basis is a propelling agent.
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| CN102500383A (en) * | 2011-11-23 | 2012-06-20 | 西安近代化学研究所 | Double oxide composite type super thermite and preparation method thereof |
| CN102634861A (en) * | 2012-04-17 | 2012-08-15 | 中国工程物理研究院化工材料研究所 | Energetic microfiber and preparation method thereof |
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| CN109796810A (en) * | 2018-12-28 | 2019-05-24 | 南京理工大学工程技术研究院有限公司 | Al-Pb for 3D printing device containing energy3O4Ink containing energy and preparation method thereof |
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| CN102500383A (en) * | 2011-11-23 | 2012-06-20 | 西安近代化学研究所 | Double oxide composite type super thermite and preparation method thereof |
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| CN104628498A (en) * | 2015-02-12 | 2015-05-20 | 西安近代化学研究所 | Energetic polyoxide compound super-thermite and preparation method thereof |
| CN104975253A (en) * | 2015-06-10 | 2015-10-14 | 陈新棠 | Thermite for composite copper pipe |
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