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ATOM PROBE TOMOGRAPHY OF REDUCED PHASES IN APOLLO 16 REGOLITH SAMPLE 61501,22

机译:APOLLO 16 REGOLITH样品中还原相的原子探针层析成像61501,22

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Nanophase iron (npFe) is relatively abundant in the lunar regolith and is widely believed to have formed by reduction of Fe during space weathering (micrometeorite/cosmic ray bombardment; [1]). Iron-silicides (Fe-Si) and native silicon require more reducing conditions than FeO, and though predicted to be present in the lunar regolith have only been reported from one lunar meteorite and one lunar regolith sample [2-4]. Fe-Si and native silicon are only stable at extremely reducing conditions and have been proposed to form by a mechanism similar to that of metallic iron [3]. The stability of native silicon requires ten orders of magnitude lower oxygen fugacity than metallic iron at temperatures above 1,600 K [5]. An early study of the soil sample (61500, [6]) suggested elevated levels of carbon, and an EPMA study of the Fe-Si from this soil sample [7] suggested that carbon might be present in the Fe-Si. Because carbon is highly reducing at the high temperatures and low pressures that would have been present during the formation of these phases, the presence of carbon was hypothesized to explain these ultra-reduced phases. In order to determine with more certainty the presence of carbon in these phases, we conducted an atom probe tomography (APT) study of Fe-Si. A representative Fe-Si bearing grain was selected and a focussed ion beam (FIB) lift-out of a Fe-Si rich region of that grain taken. The largest Fe-Si particle from the lift-out region was previously analysed with low keV EPMA [7], and served as a control for the data quality of the APT dataset. Two successful APT datasets were acquired from the FIB lift-out (Fig. 1). The first dataset (M3) was from the centre of the large (~2 μm) Fe-Si particle that was also analysed via EPMA. The major elemental chemistry as determined by APT of this sample was within 1 at% for all elements, which boosted our confidence in the quality of both the EPMA and APT data. The second dataset (M9) is from the edge of one of the smaller Fe-Si particle, and contains the boundary with the host material. Interestingly, both datasets show similar levels (~60 ppm) of carbon. However, while carbon (and indeed all of the trace elements) are homogenously distributed throughout M3, dataset M9 shows enrichment of carbon, phosphorous, nickel, chromium, cobalt, and strontium near the boundary to the host. The segregation of the trace elements towards the Fe-Si grain boundary shows that these phases did not fully quench, but does not fully constrain the timing of crystallisation. The presence of carbon within the Fe-Si raises the possibility that carbon was present during the formation of these phases, and indeed could be in-part responsible for achieving the extremely low fO_2 required to form Si metal and Fe-Si. Because the formation mechanisms for Fe-Si and npFe are hypothesized to be related, further study of npFe is warranted to investigate the similarities and differences between Fe-Si and npFe at the nanoscale. It would be interesting to see if similar trace levels of carbon or regions of trace element segregation within npFe can be visualised with APT.
机译:纳米相铁(npFe)在月球长石中相对丰富,被广泛认为是由太空风化过程中的铁还原形成的(微陨石/宇宙射线轰击; [1])。铁硅化物(Fe-Si)和天然硅比FeO需要更多的还原条件,尽管据预测在月球白云母中存在,但仅从一种月球陨石和一个月球白云母样品中报道[2-4]。 Fe-Si和天然硅仅在极度还原的条件下才稳定,并已提出通过类似于金属铁的机理形成[3]。在1600 K以上的温度下,天然硅的稳定性要求比金属铁低10个数量级的氧逸度[5]。早期对土壤样品的研究(61500,[6])表明碳含量较高,而EPMA对这种土壤样品中的Fe-Si的研究结果[7]表明,Fe-Si中可能存在碳。由于碳在这些相的形成过程中会在高温和低压下高度还原,因此假设存在碳可以解释这些超还原相。为了更确定地确定这些相中碳的存在,我们对Fe-Si进行了原子探针层析成像(APT)研究。选择了具有代表性的含Fe-Si的晶粒,并从该晶粒的富含Fe-Si的区域中取出聚焦离子束(FIB)。先前使用低keV EPMA分析了来自抬升区域的最大Fe-Si颗粒[7],并用作APT数据集​​数据质量的对照。从FIB提升中获得了两个成功的APT数据集​​(图1)。第一个数据集(M3)来自大型(〜2μm)Fe-Si颗粒的中心,该颗粒也通过EPMA分析。 APT测定的所有元素的主要元素化学组成均在1 at%以内,这增强了我们对EPMA和APT数据质量的信心。第二个数据集(M9)来自较小的Fe-Si粒子之一的边缘,并包含与主体材料的边界。有趣的是,两个数据集都显示出相似的碳水平(〜60 ppm)。但是,尽管碳(实际上是所有微量元素)均匀地分布在整个M3中,但数据集M9显示了在与宿主边界附近的碳,磷,镍,铬,钴和锶的富集。微量元素向Fe-Si晶界的偏析表明,这些相没有完全淬火,但没有完全限制结晶时间。 Fe-Si中碳的存在增加了在这些相的形成过程中存在碳的可能性,并且确实可能​​部分原因是获得了形成硅金属和Fe-Si所需的极低的fO_2。由于假设Fe-Si和npFe的形成机理是相关的,因此有必要进一步研究npFe,以研究纳米尺度下Fe-Si和npFe之间的异同。有趣的是,是否可以使用APT看到类似的痕量碳或npFe中痕量元素偏析的区域。

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