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首页> 外文期刊>Journal of Materials Science. Materials in Electronics >Synthesis and characterization of nm-sized PbTiO3 crystallites
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Synthesis and characterization of nm-sized PbTiO3 crystallites

机译：纳米级PbTiO3晶体的合成与表征

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In this work attempt is made to synthesize PbTiO3(PT) nanopowder by low temperature direct synthesis (LTDS) method already introduced by Wada et al. [8]. Various samples were prepared by precipitating a strong acidic Ti-bearing solution in an alkaline solution obtained by dissolution of Pb(NO3)(2) in a KOH solution (pH = 14). The samples were synthesized with varying Pb/Ti atomic ratios (1.0, 2.7, 6.5 and 10) at 70 degrees C. XRD, TEM, FTIR and DTA/TG techniques were utilized to characterize the obtained powders. The formation of single phase PT was not confirmed for the non-heat treated as precipitated samples in contrast with the results obtained by Wada et al. [8] for BaTiO3. Further, for the as precipitated samples not subjected to washing process with a Pb/Ti ratio above 1, the formation of unknown crystalline phase/s was detected due to the reaction taken place between Ti-bearing solution and potassium plumbate formed by dissolution of Pb(NO3)(2) in KOH solution. Applying washing process for these samples gave rise to the partial destruction of the observed structure/s and the formation of an amorphous phase as confirmed by XRD and TEM results. However, calcination of the as precipitated/washed samples at 500 degrees C and 700 degrees C for 1 hour gave rise to the formation of PT nanopowder as the main phase with average crystallite sizes in the range of about 11-14.5 nm respectively. Single phase PT nanopowder of an average crystallite size of 13 nm was formed for the sample with a Pb/Ti ratio = 1 when calcined at 500 degrees C for 1 hour. For the calcined samples with Pb/Ti ratios above 1 the formation of PbO as the second phase, however, was also detected and its level of formation was found to be related to the Pb/Ti ratio.
机译：在这项工作中，试图通过Wada等人已经介绍的低温直接合成（LTDS）方法合成PbTiO3（PT）纳米粉。 [8]。通过将强酸性含钛溶液在碱性溶液中沉淀制备各种样品，该碱性溶液是通过将Pb（NO3）（2）溶解在KOH溶液（pH = 14）中获得的。在70摄氏度下以不同的Pb / Ti原子比（1.0、2.7、6.5和10）合成样品。利用XRD，TEM，FTIR和DTA / TG技术表征所得粉末。与Wada等人获得的结果相反，对于未经热处理的沉淀样品，未确认单相PT的形成。 [8]为BaTiO3。此外，对于未经过洗涤处理且Pb / Ti比大于1的沉淀样品，由于在含Ti溶液和Pb溶解形成的铅酸钾之间发生反应，因此检测到未知的结晶相/秒的形成。 （NO3）（2）在KOH溶液中。通过XRD和TEM结果证实，对这些样品进行洗涤处理会导致观察到的结构部分破坏，并形成无定形相。然而，将沉淀/洗涤后的样品在500℃和700℃下煅烧1小时导致形成PT纳米粉作为主相，其平均微晶尺寸分别在约11-14.5nm的范围内。当在500摄氏度下煅烧1小时时，Pb / Ti比= 1的样品形成了平均微晶尺寸为13 nm的单相PT纳米粉。然而，对于Pb / Ti比大于1的煅烧样品，也检测到PbO作为第二相的形成，并且发现其形成水平与Pb / Ti比有关。

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