BaPbO_3/2024Al复合材料的制备与BaPbO_3颗粒包覆工艺的研究
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摘要
采用BaPbO_3颗粒和2024铝合金,用粉末冶金技术制备了具有辐射防护功能的BaPbO_3/2024Al复合材料。探索了复合材料的制备工艺;利用XRD、SEM和室温拉伸试验对复合材料的组织和性能进行了研究。同时探索了溶胶-凝胶法、沉淀法和室温固相反应法在BaPbO_3颗粒表面包覆Al_2O_3涂层的涂覆工艺;利用XRD、SEM、EDS和TG/DTA分析手段对包覆层和包覆效果进行了分析。
试验结果表明:制备的430℃挤压态BaPbO_3/2024Al复合材料抗拉强度可达317Mpa,但复合材料中存在Pb,说明在材料的制备过程中,BaPbO_3与2024Al基体发生反应生成了Pb;在热压温度为430℃时,热压压力为0MPa下,没有发现Pb的生成;但当存在压力时,即使温度降低为400℃依然发生反应生成了Pb,压力促进了反应,并且400℃热压态复合材料不致密。说明为了保证制备出致密的复合材料,通过控制热压温度和热压压力无法避免复合材料中界面反应的发生。
在铝溶胶浓度为0.4mol/L,Al_2O_3:BaPbO_3(wt.%)=1:1,pH=3.5-4.1,搅拌时间为30min的工艺条件下,制备出了表面被完全包覆的Al_2O_3涂层,但溶胶-凝胶法包覆Al_2O_3涂层BaPbO_3颗粒中含有氧化铅。
沉淀法在BaPbO_3颗粒上包覆Al_2O_3涂层的分析表明:只能将BaPbO_3粉末直接加入到Al(OH)3沉淀中,而不能将硝酸铝溶液加入到碱性的BaPbO_3悬浮液中;随着Al_2O_3与BaPbO_3的重量比(Al_2O_3:BaPbO_3 (wt.%))的增大,包覆效果越好;但沉淀法制备的氧化铝涂层不能完全包覆在BaPbO_3颗粒表面。
利用室温固相反应法在BaPbO_3颗粒表面完全包覆Al_2O_3涂层。EDS分析表明:颗粒的表面元素有Al元素,这证明包覆层为Al_2O_3;同时由2024Al与室温固相反应法制得的混合粉末的DTA分析可知,在350℃和500℃之间并无明显的放热和吸热峰,这说明BaPbO_3颗粒表面被完全包覆上氧化铝,氧化铝涂层防止了BaPbO_3颗粒与2024Al的接触,使反应无法进行。
The aluminium matrix composites with radioprotection function were fabricated by powder metallurgy using BaPbO_3 powders and 2024Al powders. Preparation technology is studied on impacting interface reaction of composites. The microstructure and properties of the composites were investigated by XRD, SEM and tensile test. The technical parameter is researched on making BaPbO_3 coated by Al_2O_3. The effect of coatings is investigated by XRD, SEM, EDS and TG/DTA.
The experimental results indicated that the tensile test shows that the tensile strength of the aluminium matrix composites is 317MPa, and the composites contain Pb, so there are reactions between BaPbO_3 and 2024Al when the composites were fabricated. When the sintering temperature is 430℃and no pressure, there is no reaction between BaPbO_3 and 2024Al, but when the pressure of hot pressing is not 0MPa, even if the temperature is 400℃, there also exit reactions between BaPbO_3 and 2024Al. And composite is unsound. So that shows us for making dense composites, interface reaction did not avoid through controlling the temperature and pressure of hot pressing.
When technical parameters are that concentration of Al-sol is 0.4mol/L,Al_2O_3:BaPbO_3 (wt.%)=1:1, pH=3.5-4.1 and mixed for 30min, Al_2O_3 completely coated BaPbO_3 are produced. But PbO is found in BaPbO_3 coated by Al_2O_3.
BaPbO_3 coated by Al_2O_3 are produced using chemical precipitation method. There only puting BaPbO_3 powders into Al(OH)3 liquor is suitable, and putting Al(NO3)3 liquor into BaPbO_3 suspending liquid is not suitable. The effect of coatings is better along with the Al_2O_3:BaPbO_3 (wt.%) lager. But Al_2O_3 coating is incomplete coated on BaPbO_3 surface.
Al_2O_3 completely coated BaPbO_3 are produced by a humid solid state reaction at room temperature. There is Al element on BaPbO_3 coated by Al_2O_3 by EDS analysis, so this proves the coating is Al_2O_3. DTA analysis of 2024Al+ BaPbO_3 coated by Al_2O_3 shows that there is no exothermic peak and endothermic peak between 350℃and 500℃, and this proves Al_2O_3 is completely coated on BaPbO_3, so contact between BaPbO_3 and 2024Al is impossible and reaction is avoided.
试验结果表明:制备的430℃挤压态BaPbO_3/2024Al复合材料抗拉强度可达317Mpa,但复合材料中存在Pb,说明在材料的制备过程中,BaPbO_3与2024Al基体发生反应生成了Pb;在热压温度为430℃时,热压压力为0MPa下,没有发现Pb的生成;但当存在压力时,即使温度降低为400℃依然发生反应生成了Pb,压力促进了反应,并且400℃热压态复合材料不致密。说明为了保证制备出致密的复合材料,通过控制热压温度和热压压力无法避免复合材料中界面反应的发生。
在铝溶胶浓度为0.4mol/L,Al_2O_3:BaPbO_3(wt.%)=1:1,pH=3.5-4.1,搅拌时间为30min的工艺条件下,制备出了表面被完全包覆的Al_2O_3涂层,但溶胶-凝胶法包覆Al_2O_3涂层BaPbO_3颗粒中含有氧化铅。
沉淀法在BaPbO_3颗粒上包覆Al_2O_3涂层的分析表明:只能将BaPbO_3粉末直接加入到Al(OH)3沉淀中,而不能将硝酸铝溶液加入到碱性的BaPbO_3悬浮液中;随着Al_2O_3与BaPbO_3的重量比(Al_2O_3:BaPbO_3 (wt.%))的增大,包覆效果越好;但沉淀法制备的氧化铝涂层不能完全包覆在BaPbO_3颗粒表面。
利用室温固相反应法在BaPbO_3颗粒表面完全包覆Al_2O_3涂层。EDS分析表明:颗粒的表面元素有Al元素,这证明包覆层为Al_2O_3;同时由2024Al与室温固相反应法制得的混合粉末的DTA分析可知,在350℃和500℃之间并无明显的放热和吸热峰,这说明BaPbO_3颗粒表面被完全包覆上氧化铝,氧化铝涂层防止了BaPbO_3颗粒与2024Al的接触,使反应无法进行。
The aluminium matrix composites with radioprotection function were fabricated by powder metallurgy using BaPbO_3 powders and 2024Al powders. Preparation technology is studied on impacting interface reaction of composites. The microstructure and properties of the composites were investigated by XRD, SEM and tensile test. The technical parameter is researched on making BaPbO_3 coated by Al_2O_3. The effect of coatings is investigated by XRD, SEM, EDS and TG/DTA.
The experimental results indicated that the tensile test shows that the tensile strength of the aluminium matrix composites is 317MPa, and the composites contain Pb, so there are reactions between BaPbO_3 and 2024Al when the composites were fabricated. When the sintering temperature is 430℃and no pressure, there is no reaction between BaPbO_3 and 2024Al, but when the pressure of hot pressing is not 0MPa, even if the temperature is 400℃, there also exit reactions between BaPbO_3 and 2024Al. And composite is unsound. So that shows us for making dense composites, interface reaction did not avoid through controlling the temperature and pressure of hot pressing.
When technical parameters are that concentration of Al-sol is 0.4mol/L,Al_2O_3:BaPbO_3 (wt.%)=1:1, pH=3.5-4.1 and mixed for 30min, Al_2O_3 completely coated BaPbO_3 are produced. But PbO is found in BaPbO_3 coated by Al_2O_3.
BaPbO_3 coated by Al_2O_3 are produced using chemical precipitation method. There only puting BaPbO_3 powders into Al(OH)3 liquor is suitable, and putting Al(NO3)3 liquor into BaPbO_3 suspending liquid is not suitable. The effect of coatings is better along with the Al_2O_3:BaPbO_3 (wt.%) lager. But Al_2O_3 coating is incomplete coated on BaPbO_3 surface.
Al_2O_3 completely coated BaPbO_3 are produced by a humid solid state reaction at room temperature. There is Al element on BaPbO_3 coated by Al_2O_3 by EDS analysis, so this proves the coating is Al_2O_3. DTA analysis of 2024Al+ BaPbO_3 coated by Al_2O_3 shows that there is no exothermic peak and endothermic peak between 350℃and 500℃, and this proves Al_2O_3 is completely coated on BaPbO_3, so contact between BaPbO_3 and 2024Al is impossible and reaction is avoided.
引文
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2蒋平平,沈风雷,杨春玲.防辐射有机玻璃研究现状及发展趋势.工程塑料应用. 1999,27(1):35~37
3段谨源,张兴祥,张华.防辐射纤维及材料研究的发展趋势.产业用纺织品. 1990, (5):4~8
4陈桂明,阳能军,董振旗等.一种新型核辐射防护材料的设计与应用研究.核技术. 2003,26(10):783~788
5 V.I. Kirko. Basgan: New Composite Materials for Radiation Protection. Journal of Materials Processing Technology. 2007,181:222~224
6 A.Scharmann. Past and Present of ESR in Radiation Applications. Appl.Radia.Isot. 1996,47(11):1151~1153
7 M. Durante, A. Kronenberg. Ground-based Research with Heavy Ions for Space Radiation Protection. Advances in Space Research. 2005,35:180~184
8张丹凤.中国射线防护器材的生产与管理.上海科技大学出版社, 1990:16
9李长一. X射线贯串深度等效值.钢铁研究. 1997,(1):36~40
10 A. P. Menushekov, S. Benazeth, J. Purans. Local Structure Anomalies of the BaBi(Pb)O3 System at Low Temperatures: an X-ray Absorption Study. Physic C. 1997, 277: 257~264
11 C. Mallika, G. V. Rama Rao, O. M. Sreedharan, U. V. Varadaraju. Thermodynamic Stabilities of Ternary Oxides in the Ba-Pb-O System by the e. m. f Technique. Materials Science and Engineering B.1995,33:96~102
12 W. T. Fu, D. Visser, D. J. W. Ijdo. High-resolution Neutron Powder Diffraction Study on the Structure of BaPbO3. Solid State Communications. 2005,134:647~652
13 Arlette Trokiner, Yuri Piskunov, Alexander Gerashenko, et al. Distribution of Electron Density in BaPb1-xBixO3 Evidenced by Pb and O NMR. Physica C. 2004,408~410:824~825
14梁威,杨青芳,马爱洁.防辐射纤维及材料的研究进展.中国个体防护装备. 2004,6:19~20
15许元巨.电离和电磁辐射防护材料的开发.产品用纺织品. 1995, 21(5): 41~44
16王振华.辐射防护铝基复合材料的制备工艺及性能的研究.哈尔滨工业大学工学硕士论文. 2005:1~3
17贾华明,齐鲁.防辐射纤维及其织物的研究进展.合成纤维工业. 2005,28(5):30~33
18祈章年.载人航天的辐射防护与检测.国防工业出版社, 2003:11~12
19冯玉杰.新型辐射防护材料的研究.哈尔滨工业大学工学博士论文. 1996: 13~16
20张兴祥,齐鲁,王学晨等.防X射线纤维及织物的研制与性能的研究.中国安全科学学报. 1996,6(2):22~27
21李德安,刘颖,杨文锋,杨林,李军,李梦.新型铅基复合屏蔽材料组织结构与性能.材料导报. 2006,20(10):154~158
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