LIEC, Department of Chemistry, Federal University of São Carlos, C. Postal 676, 13565-905 São Carlos, SP, Brazil.
J Colloid Interface Sci. 2010 Mar 1;343(1):256-62. doi: 10.1016/j.jcis.2009.11.027. Epub 2009 Nov 16.
Four aluminas were used as supports for impregnation with a zirconium oxide with the aim to achieve a coating, without phase separation, between support and modifier. The supports were impregnated with different concentrations of zirconium aqueous resin, obtained through the polymeric precursor method. After impregnation the samples were calcined and then characterized by XRD, which led to identification of crystalline zirconia in different concentrations from each support used. Using a simple geometric model the maximum amount of surface modifier oxide required for the complete coating of a support with a layer of unit cells was estimated. According to this estimate, only the support should be identified below the limit proposed and crystalline zirconium oxide should be identified above this limit when a complete coating is reached. The results obtained from XRD agree with the estimated values and to confirm the coating, the samples were also characterized by EDS/STEM, HRTEM, XPS, and XAS. The results showed that the zirconium oxide on the surface of alumina support reached the coating in the limit of 15 Zr nm(-2), without the formation of the ZrO(2) phase.
四种氧化铝被用作浸渍氧化锆的载体,目的是在载体和改性剂之间实现无相分离的涂层。载体用不同浓度的锆水溶胶浸渍,该溶胶通过聚合前体法获得。浸渍后,样品进行煅烧,然后通过 XRD 进行表征,从每种使用的载体中鉴定出不同浓度的结晶氧化锆。使用简单的几何模型,估算了为用单层单元完全涂覆载体所需的表面改性剂氧化物的最大量。根据该估算,当达到完全涂层时,只有在低于所提出的限制下才能识别出载体,而在高于该限制时应识别出结晶氧化锆。XRD 得到的结果与估算值一致,为了确认涂层,还通过 EDS/STEM、HRTEM、XPS 和 XAS 对样品进行了表征。结果表明,氧化铝载体表面的氧化锆在 15 Zr nm(-2) 的限制内达到了涂层,而没有形成 ZrO(2)相。