Synthesis and Dimension Control of Ultrafine γ-Aluminum Oxide by Detonation R. Y. Li1, X. J. Li, H. H. Yan, X. H. Xie, Y. D. Qu, Z. R. Yang State Key Lab of Structural Analysis for Industrial Equipment, Dept. of Engineering Mechanics, Dalian University of Technology Dalian, 116025 Abstract Ultrafine spherical γ-Aluminum Oxide was successfully obtained by detonation of the mixed explosive made by aluminum nitrate and cyclotrimethylenetrinitramine (RDX). In order to research the relation between dimension of ultrafine γ-Aluminum Oxide and explosion velocity of mixed explosive, the four mixed explosives with different explosion velocities were made. They were detonated in a container in turn, and then the four γ-Aluminum Oxide powders were prepared by their detonations. They were studied systematically by X-ray diffraction. According to XRD data, the average granule dimensions of four ultrafine γ-aluminum oxides were worked out by Scherrer formula. Comparing the average granule dimensions with explosion velocities of four mixed explosives indicated the average granule dimension was thinner when explosion velocity was higher. The relation between them was linear inverse ratio approximately. 1. Introduction At present, there are so many methods reported to synthesize ultrafine aluminum oxide [1~11], the usual employed methods are mechanical comminution, high-energy ball milling [5], chemical precipitation [6,7], pyrogenation [8,9] and sol-gel technology [10,11] etc. Each method has its characteristics. We have successfully prepared ultrafine γ-aluminum oxide which granule dimension varied from 15nm to 20nm by detonation of binary mixed explosive. Up to now, there have been not other persons who prepared ultrafine aluminum oxide by detonation at home. Some articles have only been published about nano-diamond by detonation [12~18]. The person A. A. Bukaemskii1 [19~21] has used detonation to synthesize ultrafine aluminum oxide abroad. The theory is in an oxygen-containing medium the aluminum powders were heated and drove by explosive, and then the hot and high-speed aluminum granule reacted with outer oxygen to obtain the ultrafine aluminum oxide. But ours is aluminum nitrate rapidly decomposed to large numbers of free atoms because of the high temperature (2000~3000K) and high pressure (20~30Gpa) produced by explosive, then the free aluminum atoms and oxygen atoms combined to ultrafine aluminum oxide. The method has some excellencies, such as simple technology process, low-cost equipment, fast synthesis and amplificatory yield. In addition, it has the characteristics of vapor phase composition, to synthesize high dispersing and high-purity ultrafine aluminum oxide has technique 1 Corresponding author. Tel. :+86-0411-84833303, E-mail address: [email protected] (R. Y. Li) advantage. So the method has definite value of research. At present researchers can not control the dimension of nano-material very well during its preparation. So we have done some research about controlling nano-dimension. In the experiment, we successfully changed the dimension distribution of ultrafine aluminum oxide synthesized by detonation of the binary mixed explosives through changing the velocity of explosion. And we found an organic relation between dimension of nano-granule and velocity of explosion. Sequentially in definite range, we can control the dimension of nano-material initiatively. In the experiment we changed the velocity of explosion by altering the quality of RDX among the binary mixed explosive. 2. Experiment The primary materials of four binary mixed explosives are aluminum nitrate powder and RDX powder. In the experiment, aluminum nitrate and RDX are necessary experiment materials because the ultrafine aluminum oxide is from heat decomposition of the aluminum nitrate, and RDX named as sensitizer is the condition of heat decomposition as well as. The velocity of explosion is different when the mass of RDX is different in the binary mixed explosive. To achieve different explosive with different velocity of explosion, four binary compositions containing aluminum nitrate and RDX (800g and 200g, 700g and 300g, 600g and 400g, 500g and 500g) were chosen. According to the design of experiment we weighed up the quantitative aluminum nitrate and RDX to blend them uniformly, and then put them into a hard-plastic column with a diameter of 65 mm (Fig.1) to form the columned explosive. Fig.1. Schematic diagram of columned explosive The four columned explosives were sequentially put into the explosion vessel with a diameter of 3000 mm (Fig.2) to be detonated by primers and a little plastic-type explosive (detonated powder). After every explosion, the white-gray powder was collected through the exhaust hole by the tailor-made equipment of collection.The apparatus (BC-3) was employed to measure the actual velocities of explosion of four binary mixed explosives. The synthesized products were characterized by X-ray diffraction (XRD) at a scanning rate of 4°/m (Cu-Kα, λ=0.15406nm). The morphology and particle size of ultrafine aluminum oxide were determined using a transmission electron microscope at an accelerating voltage of 100kV. Fig.2. Schematic diagram of explosion vessel 3. Results and Discussion Fig.3. Typical photographs of ultrafine aluminum oxides obtained by four binary mixtures: 500g and 500g (a); 600g and 400g (b); 700g and 300g (c); 800g and 200g (d) in turn. Fig.3 shows the transmission electron microscope photos of ultrafine aluminum oxides obtained by four binary binary mixed explosives. From photos we can see that the granules of ultrafine aluminum oxide are spherical and homogeneous, the dimensions of granules approximately varied from 15nm to 20nm. Fig.4. X-ray diffraction patterns of aluminum oxides obtained by four binary mixtures: 500g and 500g (a); 600g and 400g (b); 700g and 300g (c); 800g and 200g (d) in turn. Fig.4 shows the X-ray diffraction patterns of ultrafine aluminum oxide obtained by four binary binary mixed explosives. From patterns we can see that the shapes of four diffraction curves are same. For each diffraction curve, the three main peaks at 66.87°, 45.847°and 37.63° corresponding to the three distances of crystal faces (440), (400) and (311) are 1.39Å, 1.981Å and 2.38Å, and other two little peaks at 39.45° and 60.87° which corresponding to the two distances of crystal faces are 2.28Å and 1.52Å. According to ASTM catalog data, the bove data completely accord with the standard data of γ-aluminum oxide. So we can conclude that the four groups of white-gray powder are all γ-aluminum oxide powder. In addition, the average granule dimension (D) of ultrafine aluminum oxide by detonation of every binary mixed explosive can be calculated out by Scherrer formula. The formula is following: D=kλ/Bcosθ (1) where k is a constant taken as 0.89, λ is the wavelength of Cu target taken as 0.154nm, 2θ is the scattering angle, B is the angular half-width of the peak . According to all the diffraction data, we calculated out the average granule dimensions of ultrafine aluminum oxide obtained by the four binary mixed explosives detonation by the formula (1). We can also measure out the actual velocities of explosion (V) of four binary mixed explosives by BC-3 apparatus. The calculated D and the measured V are shown in Tab.1. Tab.1 Values of D and V Binary compositions D/nm V/(m⋅s-1) 500g and 500g 15.43 5263 600g and 400g 17.11 4624 700g and 300g 19.61 3846 800g and 200g 22.96 2888 In Tab.1, we can see that the average granule dimension is more and more large from the top down, but the velocity of explosion turn more and more small. The relation between them is inverse ratio. To show the relation more distinctly we drew the following fig.5. Fig.5. Relation curve of nano-dimension and velocity of explosion Fig.5 indicates that when the velocity of explosion of binary mixed explosive is higher the average granule dimension of ultrafine aluminum oxide obtained by it is more small, the particle of ultrafine aluminum oxide is thinner i.e.. The relation is linear inverse ratio approximately. So based on the curve we can easily change the velocity of explosion to control the dimension of nano-granule initiatively in a definite range. 4. Conclusions Four binary mixed explosives with different velocities of explosion are made by aluminum nitrate and RDX at different mass ratios. Ultrafine γ-aluminum oxide is synthesized by detonation of each binary mixed explosive. The granules of ultrafine γ-aluminum oxide are spherical, the dimensions of granules approximately vary from 15nm to 20nm and the granules are homogeneous. The relation between the velocity of explosion of binary mixed explosive and granule dimension of ultrafine aluminum oxide is linear inverse ratio approximately. When the velocity of explosion of binary mixed explosive is higher the granule of ultrafine aluminum oxide by detonation is smaller. Acknowledgements The project is partially supported by the National Nature Science Foundation and the Natural Science Foundation of Liaoning Province under contract No. 10572034 and No. 20042161. References [1] Y. G. Zhan and F. Ran: Inorganic Chemicals Industry, 2001, 33(3), 19. [2] J. H. He, J. G. 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