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干法、室温振动研磨制备铝超微颗粒, 分别将研磨2 h, 4 h和8 h的铝粉, 在常温下超声水解得到白色Al(OH)3胶体, 水解产品经干燥、研磨、焙烧后制备出多孔、片状-Al2O3纳米颗粒, 粒度分布在3050 nm之间. 借助于X射线衍射(XRD)分析方法和透射电子显微镜(TEM), 研究固体颗粒在细化过程中的能量转换, 分析颗粒的微结构演化与机械力化学反应的关系, 确定理想的研磨时间. 研究结果表明: 固体颗粒在机械力的作用下产生大量的应变和位错缺陷, 使材料处于亚稳、高能活性状态, 易于诱发机械力化学反应, 在一定条件下晶体的表面能、应变能和层错能相互转化; 研磨2 h的铝颗粒内部, 晶格畸变和位错概率最大, 材料显示出极高的化学反应活性, 在超声波激发下, 储存在材料内部的能量被充分释放, 在较短的时间内, 水解生成Al(OH)3纳米颗粒.Al ultra-fine grains are prepared by dry roller vibration milling at room temperature. After the ultrasonic hydrolyzing, the Al powders are milled for 2 h, 4 h and 8 h, separately, becoming the colloidal Al(OH)3. After the hydrolyzing production are dried, grinded, calcined, the flaky -Al2O3 nano-particles are obtained, and the particles sizes are in the range from 30 to 50 nm. By X ray diffraction (XRD) analysis method and transmission electron microscope (TEM), we analyze the energy conversion of solid particles in the vibration milling, and study the relation between the structure evolvement of solid particles and mechano-chemical reaction, in order to ascertain ideal milling time. The research results indicate that the solid particles under the action of mechanical force generate a mass of deformation and dislocation flaws and the material is in metastable high-energy state, which is favorable for inducing mechano-chemical reaction. In certain conditions, the surface energy of crystalloid, strain and dislocation energy could be mutually converted. The odds of lattice distortion and dislocation are maximal for the 2 h-milled Al powders, so the material shows a higher chemical reaction activation. On the ultrasonic agitation, the energy is fully released from the material interior, then Al(OH)3 nano-particles are prepared in a short time.
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Keywords:
- vibration milling /
- structure evolvement /
- -Al2O3 /
- mechanical activation
[1] Heinicke G 1984 Tribochemistry (Berlin: Akademie-Verlag) p11---17
[2] Chen D, Chen Z H 2008 Mechanical Force Chemistry (Beijing: Chemical Industry Press) p1---36 (in Chinese) [陈鼎, 陈振华 2008 机械力化学 (北京:化学工业出版社) 第1---36页]
[3] Thompson J R 1987 Europhysics Letters 55 117
[4] Schlump W 1989 New Materials by Mechanical Alloy Technology (Oberursel: DGM Informations Gesellschaft) p307
[5] Kishimura H, Matsumoto H 2011 Journal of Alloys and Compound 509 4386
[6] Xue J M, Zhou Z H, Wang J 2002 Materials Chemistry and Physics 75 81
[7] Lubomirsky I 2006 Solid State Ionics 177 1639
[8] Dong H N, Wu X X, Wu S Y, Zheng W C 2002 Acta Phys. Sin. 51 616 (in Chinese) [董会宁, 吴晓轩, 邬劭轶, 郑文琛 2002 51 616]
[9] Wang S L 2002 Progress in Natural Science 2 336
[10] Pu Z H, Yang C Z, Qin P, Lou Y W 2008 Powder Diffraction 23 213
[11] Qin P, Lou Y W, Yang C Z, Xia B J 2006 Acta Phys. Sin. 55 1325 (in Chinese) [钦佩, 娄豫皖, 杨传铮, 夏保佳 2006 55 1325]
[12] Kostic E, Kiss S, Boskovic S, Zec S 1997 Powder Technology 91 49
[13] Yuan T C, Cao Q Y, Li J 2010 Hydrometallurgy 104 136
[14] Kumar S, Kumar R 2011 Ceramics International 37 533
[15] Tkácová K, Heegn H, Stevulová N 1993 International Journal of Mineral Processing 40 17
[16] Liu L W, Tan L, Huang G 2011 Chin. Phys. B 20 1
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[1] Heinicke G 1984 Tribochemistry (Berlin: Akademie-Verlag) p11---17
[2] Chen D, Chen Z H 2008 Mechanical Force Chemistry (Beijing: Chemical Industry Press) p1---36 (in Chinese) [陈鼎, 陈振华 2008 机械力化学 (北京:化学工业出版社) 第1---36页]
[3] Thompson J R 1987 Europhysics Letters 55 117
[4] Schlump W 1989 New Materials by Mechanical Alloy Technology (Oberursel: DGM Informations Gesellschaft) p307
[5] Kishimura H, Matsumoto H 2011 Journal of Alloys and Compound 509 4386
[6] Xue J M, Zhou Z H, Wang J 2002 Materials Chemistry and Physics 75 81
[7] Lubomirsky I 2006 Solid State Ionics 177 1639
[8] Dong H N, Wu X X, Wu S Y, Zheng W C 2002 Acta Phys. Sin. 51 616 (in Chinese) [董会宁, 吴晓轩, 邬劭轶, 郑文琛 2002 51 616]
[9] Wang S L 2002 Progress in Natural Science 2 336
[10] Pu Z H, Yang C Z, Qin P, Lou Y W 2008 Powder Diffraction 23 213
[11] Qin P, Lou Y W, Yang C Z, Xia B J 2006 Acta Phys. Sin. 55 1325 (in Chinese) [钦佩, 娄豫皖, 杨传铮, 夏保佳 2006 55 1325]
[12] Kostic E, Kiss S, Boskovic S, Zec S 1997 Powder Technology 91 49
[13] Yuan T C, Cao Q Y, Li J 2010 Hydrometallurgy 104 136
[14] Kumar S, Kumar R 2011 Ceramics International 37 533
[15] Tkácová K, Heegn H, Stevulová N 1993 International Journal of Mineral Processing 40 17
[16] Liu L W, Tan L, Huang G 2011 Chin. Phys. B 20 1
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