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Twins within platinum and palladium films on YSZ-Location for hole formation during de-wetting and oxygen exchange

机译:YSZ上铂和钯薄膜中的孪晶,用于在去湿和氧气交换过程中形成孔

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摘要

Platinum and Palladium films were prepared on (111) orientated yttrium-stabilised zirconia (YSZ) by pulsed laser deposition (PLD). Afterwards, the Pt/YSZ and Pd/YSZ systems were annealed and/or electrically polarised. The polarisation was performed in the manner that oxygen was alternatingly built-out and built-in (= cyclovoltammetry experiment) at and within the metal films. The as-deposited, annealed and polarised films, respectively, were characterised by EBSD, SEM, X-ray pattern and pole figure measurements. In addition, the X-ray patterns were measured in situ during annealing and during polarisation. The as-deposited metal films were nearly single crystalline, but with twins of a size between 100 nm and 300 nm as defects. These twins disappear completely during annealing in platinum films on perfect (111) orientated YSZ single crystals and holes are built instead. Whereas-at least a small fraction of-twins remains in films on twin-rich YSZ(111) substrates. Nevertheless, during polarisation these twins also disappear completely, probably due to formation and cracking of oxygen bubbles at twin positions within the metal films. Palladium films behave similarly, but they show stronger de-wetting phenomenon during annealing. They are also oxidised during annealing at an oxygen partial pressure [= p(O _2)] above 1·10 ~(- 3) mbar at temperatures between 500 °C and 700°C or even at this low p(O _2) after some hours at 500°C. During polarisation they are even oxidised at 400°C at p(O _2) > 1·10 ~(- 3) mbar.
机译:通过脉冲激光沉积(PLD)在(111)取向的钇稳定氧化锆(YSZ)上制备了铂和钯薄膜。之后,对Pt / YSZ和Pd / YSZ系统进行退火和/或电极化。以这样的方式进行极化:在金属膜上和金属膜内交替地内建和内建氧气(=伏安法实验)。通过EBSD,SEM,X射线图和极图测量分别表征沉积后的薄膜,退火薄膜和偏光薄膜。另外,在退火期间和极化期间原位测量X射线图案。所沉积的金属膜几乎是单晶的,但是具有在100nm至300nm之间的尺寸的孪晶作为缺陷。这些孪晶在退火过程中在完美(111)取向的YSZ单晶上的铂膜中完全消失,并代之以孔。而至少一小部分的孪晶保留在富含孪晶的YSZ(111)基材上的薄膜中。然而,在极化过程中,这些孪晶也完全消失了,这可能是由于在金属膜中的孪晶位置处的氧气气泡的形成和破裂。钯膜的行为类似,但是在退火过程中它们显示出更强的去湿现象。它们还会在退火过程中,在500°C至700°C的温度下,甚至在如此低的p(O _2)之后,在高于1·10〜(-3)mbar的氧分压[= p(O _2)]时被氧化。在500°C下几个小时。在极化过程中,它们甚至在p(O _2)> 1·10〜(-3)mbar下于400°C氧化。

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