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Effect of sintering time on structural, microstructural and chemical composition of Ni-doped lanthanum gallate perovskites

机译:烧结时间对掺镍没食子酸镧钙钛矿结构,微结构和化学成分的影响

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This work reports the effect of two different sintering times, 6 and 48 h on the structural, microstructural, and chemical features of Ni-doped La0.90Sr0.10GaO3.00-delta. Independently of the sintering time, La0.90Sr0.10Ga1-xNixO3.00-delta (where x=0.10, and 0.20 (mol)) presents a rhombohedral symmetry with a lattice volume that decreases when NiO dopant increases. Besides the perovskite, LaSrGa3.00O7.00 (nominal composition) is present as second phase in all cases. When the samples are doped with NiO, the peaks of this second phase are shifted with respect to the peaks of the pure phase. These shifts suggest that this second phase could admit some Ni ions in its structure. According to the XRD patterns, the amount of the latter phase is larger when sintering time is increased. Electron probe microanalysis (EPMA) indicated that the matrix of the samples sintered for 6 h is constituted by a perovskite with an experimental composition very close to the nominal one. However, when the samples are sintered for 48 h the matrix of each sample is constituted by two perovskites; both with compositional deviations with respect to their nominal one. In particular, a significant Sr depletion compensated by a La increment in the A site is observed. Those compositional deviations could be mainly due to the diffusion of the cations in the bulk and/or from the bulk to the surface of the samples. That diffusion can favour the formation, not only, of a second perovskite with a different composition in relation with the first one formed, but also, the formation of second phases. In addition, a very slight broadening of Bragg peaks of the perovskites sintered for 48 h is observed by XRD and can be related to the presence of two different perovskites in each sample according to EPMA results.
机译:这项工作报告了两个不同的烧结时间(6和48 h)对掺Ni的La0.90Sr0.10GaO3.00-δ的结构,微观结构和化学特性的影响。与烧结时间无关,La0.90Sr0.10Ga1-xNixO3.00-δ(其中x = 0.10和0.20(mol))呈现菱面体对称性,其晶格体积随NiO掺杂剂的增加而减小。除钙钛矿外,LaSrGa3.00O7.00(名义组成)在所有情况下均作为第二相存在。当样品中掺杂有NiO时,第二相的峰相对于纯相的峰发生位移。这些变化表明,第二相可以在其结构中吸收一些镍离子。根据XRD图谱,当增加烧结时间时,后相的量较大。电子探针微分析(EPMA)表明,烧结6 h的样品基质由钙钛矿构成,其钙钛矿的实验组成非常接近标称值。但是,将样品烧结48小时后,每个样品的基质都由两个钙钛矿组成。两者均相对于其标称值之一具有成分偏差。特别地,观察到由A位中的La增量补偿的显着的Sr耗尽。这些组成偏差可能主要是由于阳离子在本体中和/或从本体到样品表面的扩散所致。该扩散不仅有利于形成具有与所形成的第一钙钛矿不同的组成的第二钙钛矿,而且有利于第二相的形成。此外,通过XRD观察到,烧结48h的钙钛矿的布拉格峰非常轻微的增宽,根据EPMA结果,这可能与每个样品中存在两种不同的钙钛矿有关。

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