CN102500383A - Double oxide composite type super thermite and preparation method thereof - Google Patents
Double oxide composite type super thermite and preparation method thereof Download PDFInfo
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- CN102500383A CN102500383A CN2011103740659A CN201110374065A CN102500383A CN 102500383 A CN102500383 A CN 102500383A CN 2011103740659 A CN2011103740659 A CN 2011103740659A CN 201110374065 A CN201110374065 A CN 201110374065A CN 102500383 A CN102500383 A CN 102500383A
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Abstract
The invention discloses a double oxide composite type super thermite. The double oxide composite type super thermite comprises the following components in part by weight: 1 to 4 parts of Al powder, 1 to 8 parts of CuO and 1 to 8 parts of MxOy, wherein the MxOy is a metal oxide; M is selected from the II-th, the III-th, the IV-th and the V-th main group metal elements, transition metal elements or lanthanide elements; M is not Cu; x and y are positive integers and meet chemically reasonable values; and the grain size of the aluminum powder is 20 to 100 nm. The double oxide composite type super thermite has small grain size and high purity, serves as a combustion catalyst, has an excellent catalytic effect on combustion of a double-base propellant, and can remarkably increase the combustion speed of the propellant and reduce the pressure index.
Description
Technical field
The present invention relates to compound super thermite of a kind of double oxide and preparation method thereof; This contains and can compound thermite can be used as double-basis is propellant burning catalyst; The double-basis that is mainly used in guided missile, rocket is propellant loading, belongs to the nano material preparation technical field.
Background technology
Double-basis is that propellant is the one type of high-energy fuel that is used for rocket and guided missile, but its shortcoming is that combustion speed is lower, pressure index is higher, needs to add combustion catalyst and regulates combustibility.Discover that double-basis is that propellant generation hypervelocity combustion phenomena is relevant with the burningrate catalyst granule size, specific surface area of catalyst is bigger, activity is high more, and its combustion catalysis effect is just obvious more.Therefore nm-class catalyst shows huge superiority and good application prospect because its specific area is big, specific surface energy is high and the active height of specific surface brings higher catalytic efficiency in the catalytic combustion of propellant.Research also finds, single catalyst is that the combustibility of propellant makes moderate progress to double-basis, but effect is not remarkable, and compounded catalyst is because its " cooperative effect " can be optimized the combustibility that double-basis is a propellant greatly.For example, lead-copper-carbon is deceived three's compound use under certain ratio, occurs pressure index when the RDX-Al-CMDB propellant burning rate is improved less than 0.3 good result, even also can realize " platform " or " wheat is spread " aptitude to burn.
Along with the continuous development improvement of rocket-powered missile technology, it is to power source---and the requirement of propellant is also increasingly high, therefore needs the efficient burning catalyst of development of new to satisfy the needs that the novel solid propellant develops.In addition, double-basis is the power source of propellant as rocket and guided missile, and it must pursue higher energy.Though yet the use of inert catalyst has improved the combustibility of propellant, also reduced its energy simultaneously.Therefore, exploration and exploitation contain can just become an important directions in the research of novel solid propellant by burningrate catalyst.The important feature that contains the ability catalyst is exactly itself to contain ability; Can contain can group or realize by containing methods such as can component forming composite catalyst through introducing in the catalyst molecule; It is both can be collaborative improving combustibility 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 propellant.
Nanometer aluminium powder is applied in the solid propellant as high-energy fuel, has been proved to be to improve propellant burning property widely, can significantly promote solid propellant combustion rate and reduce burning rate pressure exponent.Yet; The incompatibility of nanometer aluminium powder and organic solvent reaches and in air, acid, alkaline medium, is corroded easily; High reactivity causes its easy reunion and surface to be prone to oxidized and loses activity; Its practical application in propellant is had a greatly reduced quality, therefore to the surface modification of nanometer aluminium powder, the focus that active protection has become current research.The reactive systems of the nano level metal base energetic material that obtains through Combined Processing by nanometer aluminium powder and metal oxide; Be called super thermite (Super Thermites) or the intermolecular compound of metastable state (Metastable Intermolecular Composites; MIC); It can bring following benefit as the combustion catalyst expectation: first; Weaken even eliminate nanometer aluminium powder, improve the dispersiveness of nanometer aluminium powder effectively, thereby can guarantee giving full play to of its excellent nano functional characteristic because of the agglomeration that self motive power causes; The second, being chosen at double-basis is the nano-metal-oxide that has better catalytic effect in the propellant, can bring into play it and be applied to the excellent properties that propellant brings, and not only can improve propellant burning rate, can also reduce pressure index; The 3rd; Nano-metal-oxide and nanometer aluminium powder Combined Processing; When the protection nanometer aluminium powder is active; Can make full use of the cooperative effect of two kinds of material function property, the excellent functional characteristic of nano particle is improved greatly, give full play to its effect as the SOLID PROPELLANT COMBUSTION catalyst.
Summary of the invention
The purpose of this invention is to provide a kind of improve double-basis be containing of propellant combustion characteristic can double oxide compound super thermite, to overcome the deficiency of prior art.
Another object of the present invention is to provide the above-mentioned preparation method who contains the compound super thermite of ability double oxide.
Implementation procedure of the present invention is following:
The compound super thermite of a kind of double oxide, its composition and weight portion are:
Al powder 1-4 part
CuO 1-8 part
M
xO
y1-8 part
M
xO
yBe metal oxide, M is selected from II, III, IV, V main group metal element, transition metal or lanthanide series, and M is not Cu, and x and y are positive integer, and it satisfies chemically reasonable value, and said aluminium powder particle diameter is 20 ~ 100 nm.
Said satisfied chemically reasonable value is meant that for example when metal M was divalence Pb, x was 1, and y is 1; As when M is trivalent La, x is 2, and y is 3.
The optimum formula of the compound super thermite of above-mentioned double oxide is:
Al powder 1-4
CuO 2-6
M
xO
y 2-6。
M is preferably lead, bismuth, tin, nickel, cobalt, chromium, iron, zirconium, aluminium, magnesium, molybdenum, cadmium, manganese, titanium, vanadium, zinc, lanthanum, cerium, neodymium, europium, most preferably is lead, bismuth, tin, zirconium, cerium.
The particle diameter of the compound super thermite that obtains through method for preparing is 80 ~ 200 nm.
The preparation method of the compound super thermite of above-mentioned double oxide may further comprise the steps:
(1) soluble copper salt is dissolved in the absolute ethyl alcohol;
(2) in above-mentioned solution, add slaine proton scavengers, nanometer aluminium powder and metal oxide M
xO
y
(3) generate wet gel at 15 ~ 75 ℃;
(4) with wet gel oven dry handle xerogel, grind, calcining promptly makes product;
Above-mentioned all operations carries out under nitrogen protection.
Described soluble copper salt is copper nitrate, Schweinfurt green, copper chloride or copper sulphate; Described slaine proton scavengers is selected from 1,2-expoxy propane, 1,2-epoxy butane, epoxy prapanol, epoxychloropropane, epoxy fluoro-propane, epoxy bromopropane, epoxy hexane, butadiene monoxide, cis-2,3-butylene oxide.
Wet gel is at 50 ~ 100 ℃ of vacuum drying 20 ~ 40 h in the above-mentioned steps (4), and the calcination processing temperature is 350 ℃ ~ 550 ℃, and the processing time is 1.5 ~ 3 h.
It is as combustion catalyst in the propellant that the compound super thermite of the double oxide that the present invention prepares can be used for double-basis.
For arrival improves the requirement that double-basis is the propellant combustion characteristic; The present invention at first will solve the agglomeration traits of condensing of single nanometer combustion catalyst; Need to select a kind of can be as the metal oxide of the carrier of combustion catalyst or anticoagulant, take suitable preparation technology; So that compound super thermite active component is dispersed in the surface reaction district of flame structure in combustion process, makes it fully react the maximization that reaches catalytic effect, and be difficult for coacervating large particle or form aggregate; In addition, the metal oxide of selection also can produce " synergy " of catalytic effect with compound combustion catalyst active component.Through inventor's different metal oxides that makes repeated attempts; Find that cupric oxide possesses above-mentioned performance; And sol-gel technology occurs in the highly cross-linked three-dimensional space network " skeleton " owing to its polymerization; Can accurately control composition, carrier bore hole size, product particle size and the structure of product at nanoscale, therefore meet the requirements.
Advantage of the present invention and good effect: (1) is raw material with soluble copper salt, absolute ethyl alcohol and slaine proton scavengers, and cheap and easy acquisition adopts nontoxic absolute ethyl alcohol to make solvent, environmental nonpollution; (2) the product particle diameter is little, purity is high, is reflected at liquid-phase mixing under the ultrasound condition, and nanometer aluminium powder and nano-metal-oxide disperse better the product that finally obtains to be uniformly dispersed in gel carrier; (3) the present invention is simple to operate, and course of reaction is easy to control, and security performance is high, and manufacturing cycle is short, and is economical and practical, production cost is low, is suitable for large-scale production; (4) the present invention utilizes characteristic and the sol-gel preparation technology's of nano material advantage to solve the coagulation problems of nanometer combustion catalyst; Its active component is evenly disperseed in the propellant combustion process, thereby the catalytic activity time is long, catalytic efficiency improves; In addition, " cooperative effect " by composite catalyst improved propellant burning property greatly; (5) the compound super thermite of double oxide of the present invention is that the burning of propellant has good catalytic effect as combustion catalyst to double-basis, can significantly improve propellant burning rate and reduce pressure index.
Description of drawings
Fig. 1 is the XRD figure of the compound super thermite powder of Al/CuOPbO double oxide;
Fig. 2 is the SEM photo of the compound super thermite powder of Al/CuOPbO double oxide;
Fig. 3 is the EDS ability spectrogram of the compound super thermite powder of Al/CuOPbO double oxide;
Fig. 4 is Al/CuOBi
2O
3The XRD figure of the compound super thermite powder of double oxide;
Fig. 5 is Al/CuOBi
2O
3The SEM photo of the compound super thermite powder of double oxide;
Fig. 6 is Al/CuOBi
2O
3The EDS of the compound super thermite powder of double oxide can spectrogram.
The specific embodiment
Embodiment 1
(1) takes by weighing 2.128 g Gerhardites, under the sonic oscillation condition, it is dissolved in the 15 mL absolute ethyl alcohols fully;
(2) slow Dropwise 5 mL 1; The 2-expoxy propane is in above-mentioned suspension; Add 0.3003 g nanometer aluminium powder down in the sonic oscillation effect behind 4 min; Add subsequently the nano oxidized lead of 0.70 g (30～80nm), continuing to generate wet gel behind sonic oscillation 1 h under 48 ℃ of constant temperatures, cool off then, leave standstill;
(3) 24 h are handled in the 80 ℃ of oven dry in vacuum drying oven of the wet gel after still aging and get xerogel, the xerogel after will grinding subsequently is 439 ℃ of calcining 2.5 h in Muffle furnace, can make the compound super thermite Al/CuOPbO of double oxide.
The inventor is Al powder 1-4 part, and CuO1-8 part changes prescription in PbO 1-8 part scope, all prepare the different compound super thermites of forming.
Product characterizes with field emission scanning electron microscope-power spectrum (SEM-EDS) analysis, X-ray powder diffraction (XRD), infrared spectrometer (IR), x-ray fluorescence spectrometry (XRF) and thermogravimetric analyzer (TG) confirms its structural behaviour and composition model.
From Fig. 1 is the XRD figure of the compound super thermite powder of Al/CuOPbO double oxide; Powder diffraction result and the contrast of PDF card; Composite granule is metallic aluminium (PDF card 04-0787); Cupric oxide (PDF card 41-0254) and lead oxide (PDF card 05-0561), the interplanar distance of product feature diffraction maximum
dThe standard diagram card of Al, CuO and PbO matches in value and the standard P DF card, exists the characteristic diffraction peak of these three kinds of materials and peak shape good;
Fig. 2 shows that the nanocrystalline particle diameter of the compound super thermite of Al/CuOPbO double oxide is between 80 ~ 180 nm;
Fig. 3 EDS can O, Cu, Al, four kinds of elements of Pb occur in the spectrogram, does not have other impurity, explains and only contains O, Cu, Al, four kinds of elements of Pb in the product.
(1) takes by weighing 3.193 g Gerhardites, under the sonic oscillation condition, it is dissolved in the 15 mL absolute ethyl alcohols fully;
(2) slow Dropwise 5 mL 1; The 2-expoxy propane is in above-mentioned suspension; Add 0.3355 g nanometer aluminium powder down in the sonic oscillation effect behind 4 min; Add subsequently 1.03 g nanometer bismuth oxides (30～80nm), continuing to generate wet gel behind sonic oscillation 1 h under 52 ℃ of constant temperatures, cool off then, leave standstill;
(3) 28 h are handled in the 80 ℃ of oven dry in vacuum drying oven of the wet gel after still aging and get xerogel, the xerogel after will grinding subsequently is 445 ℃ of calcining 2.5 h in Muffle furnace, can make the compound super thermite Al/1.5CuO1.5Bi of double oxide
2O
3
The inventor is at Al powder 1-4 part, CuO1-8 part, Bi
2O
3Change prescription in 1-8 part scope, all prepared the compound super thermite of different compositions.
Product characterizes with field emission scanning electron microscope-power spectrum (SEM-EDS) analysis, X-ray powder diffraction (XRD), infrared spectrometer (IR), x-ray fluorescence spectrometry (XRF) and thermogravimetric analyzer (TG) confirms its structural behaviour and composition model.
Fig. 4 is Al/CuOBi
2O
3The X-ray diffraction result of the compound super thermite powder of double oxide; Contrast with the PDF card; Composite granule is metallic aluminium (PDF card 04-0787), cupric oxide (PDF card 41-0254) and bismuth oxide (PDF card 41-1449), the interplanar distance of product feature diffraction maximum
dAl, CuO and Bi in value and the standard P DF card
2O
3The standard diagram card match, exist the characteristic diffraction peak of these three kinds of materials and peak shape good.
Fig. 5 shows that product is equally distributed Al/CuOBi
2O
3Nanocrystalline, particle diameter is between 100 ~ 200 nm.
Fig. 6 EDS can O, Cu, Al, four kinds of elements of Bi occur in the spectrogram, does not have other impurity, explains and only contains O, Cu, Al, four kinds of elements of Bi in the product.
(1) takes by weighing 2.128 g Gerhardites, under the sonic oscillation condition, it is dissolved in the 15 mL absolute ethyl alcohols fully;
(2) slow Dropwise 5 mL epoxychloropropane is in above-mentioned suspension; Add 0.4599 g nanometer aluminium powder down in the sonic oscillation effect behind 4 min; Add 0.70 g nano-stannic oxide (30～80nm) subsequently; Continuing to generate wet gel behind sonic oscillation 1 h under 50 ℃ of constant temperatures, cool off then, leave standstill;
(3) 24 h are handled in the 80 ℃ of oven dry in vacuum drying oven of the wet gel after still aging and get xerogel, the xerogel after will grinding subsequently is 439 ℃ of calcining 2.5 h in Muffle furnace, can make the compound super thermite Al/CuOSnO of double oxide
2
The inventor is at Al powder 1-4 part, CuO1-8 part, SnO
2Change prescription in 1-8 part scope, all prepare the different compound super thermites of forming.
Product characterizes with field emission scanning electron microscope-power spectrum (SEM-EDS) analysis, X-ray powder diffraction (XRD), infrared spectrometer (IR), x-ray fluorescence spectrometry (XRF) and thermogravimetric analyzer (TG) confirms its structural behaviour and composition model.The synthetic composite oxides Al/CuOSnO that obtained of analysis result
2
Embodiment 4
Ammonium perchlorate is a kind of important propellant component; Composite oxide catalytic ammonium perchlorate (AP) thermal decomposition that this examples preparation obtains is studied; Single metal is taked the blending method preparation; Discover that the composite oxides thermite compares with corresponding single oxide, can significantly improve the thermal discharge of AP, experimental result is as shown in table 1.
Experimentation and condition are following: (table 1 numbering 2-8) is that 1:5 carries out weighing with the AP mass ratio by sample, makes sample and AP fully mix the laboratory sample of back for making the two mixed grinding; Amount of samples during test: 0.5-1.0mg; Heating rate: 10 ℃/min; Temperature range: 30-490 ℃; Atmosphere: still air atmosphere.T in the table 1
P(℃) represent decomposition peak's temperature, Δ T
p(℃) for comparing the temperature that pure AP shifts to an earlier date, the thermal discharge of Δ H (kJ/g) for amounting to.
Claims (8)
1. compound super thermite of double oxide, its composition and weight portion are:
Al powder 1-4 part
CuO 1-8 part
M
xO
y1-8 part
M
xO
yBe metal oxide, M is selected from II, III, IV, V main group metal element, transition metal or lanthanide series, and M is not Cu, and x and y are positive integer, and it satisfies chemically reasonable value, and said aluminium powder particle diameter is 20 ~ 100 nm.
2. the compound super thermite of double oxide according to claim 1 is characterized in that:
Al powder 1-4
CuO 2-6
M
xO
y 2-6。
3. the compound super thermite of double oxide according to claim 1 and 2 is characterized in that: M is lead, bismuth, tin, nickel, cobalt, chromium, iron, zirconium, aluminium, magnesium, molybdenum, cadmium, manganese, titanium, vanadium, zinc, lanthanum, cerium, neodymium, europium.
4. the compound super thermite of double oxide according to claim 3 is characterized in that: M is lead, bismuth, tin, zirconium, cerium.
5. the compound super thermite of double oxide according to claim 3 is characterized in that: the particle diameter of compound super thermite is 80 ~ 200 nm.
6. the preparation method of the compound super thermite of the said double oxide of claim 1 may further comprise the steps:
(1) soluble copper salt is dissolved in the absolute ethyl alcohol;
(2) in above-mentioned solution, add slaine proton scavengers, nanometer aluminium powder and metal oxide M
xO
y
(3) generate wet gel at 15 ~ 75 ℃;
(4) with wet gel oven dry handle xerogel, grind, calcining promptly makes product.
7. according to the preparation method of the compound super thermite of the said double oxide of claim 6, it is characterized in that: described soluble copper salt is copper nitrate, Schweinfurt green, copper chloride or copper sulphate.
8. according to the preparation method of the compound super thermite of the said double oxide of claim 6; It is characterized in that: described slaine proton scavengers is selected from 1; 2-expoxy propane, 1; 2-epoxy butane, epoxy prapanol, epoxychloropropane, epoxy fluoro-propane, epoxy bromopropane, epoxy hexane, butadiene monoxide, cis-2, the 3-butylene oxide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103264222A (en) * | 2013-05-24 | 2013-08-28 | 合肥荣事达三洋电器股份有限公司 | Welding method for aluminium wire and copper wire for motor |
| 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 |
| CN105537605A (en) * | 2016-01-12 | 2016-05-04 | 西安近代化学研究所 | Preparation method of Al/Fe2O3 thermite |
| CN110028372A (en) * | 2019-04-24 | 2019-07-19 | 中北大学 | The method for preparing Al/CuO Energetic Nanomaterials based on base catalysis sol-gal process |
| CN115141070A (en) * | 2022-07-07 | 2022-10-04 | 西南科技大学 | Nano thermite and preparation method of nano thermite micro self-destruction chip |
| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
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| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
| CN101921160A (en) * | 2010-09-14 | 2010-12-22 | 西安近代化学研究所 | Preparation method of super-thermite Al/PbO nano-composite energetic material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1513596A (en) * | 2003-07-07 | 2004-07-21 | 深圳大学 | Nano-copper-lead composite oxide powder and its preparation method |
| CN101921160A (en) * | 2010-09-14 | 2010-12-22 | 西安近代化学研究所 | Preparation method of super-thermite Al/PbO nano-composite energetic material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103264222A (en) * | 2013-05-24 | 2013-08-28 | 合肥荣事达三洋电器股份有限公司 | Welding method for aluminium wire and copper wire for motor |
| 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 |
| CN105537605A (en) * | 2016-01-12 | 2016-05-04 | 西安近代化学研究所 | Preparation method of Al/Fe2O3 thermite |
| CN110028372A (en) * | 2019-04-24 | 2019-07-19 | 中北大学 | The method for preparing Al/CuO Energetic Nanomaterials based on base catalysis sol-gal process |
| CN110028372B (en) * | 2019-04-24 | 2021-06-04 | 中北大学 | Method for preparing Al/CuO nano energetic material based on alkaline catalysis sol-gel method |
| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
| CN115141070A (en) * | 2022-07-07 | 2022-10-04 | 西南科技大学 | Nano thermite and preparation method of nano thermite micro self-destruction chip |
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