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Electrostatic levitation studies of supercooled liquids and metastable solid phases

机译:过冷液体和亚稳固相的静电悬浮研究

摘要

A new laboratory has been developed at Iowa State University (ISU) to be used for the study of high temperature liquids and solids, with particular focus on the supercooling of liquids and their metastable solidification products. This new laboratory employs the electrostatic levitation (ESL) technique, in which a charged sample is suspended between a set of electrodes to achieve non-contact handling. Owing to the elimination of a crucible, high temperature processing of samples can be achieved with reduced levels of contamination and heterogeneous nucleation. Because of the reduction in heterogeneous nucleation, samples can be supercooled well below their equilibrium melting temperature, opening the door to a wide range of measurements on supercooled liquids. Measurements methods have been implemented for the characterization of thermophysical properties such as: volume/density, ratio of specific heat to total hemispherical emissivity, surface tension, viscosity, electrical resistivity, and magnetic susceptibility. For measurements of electrical resistivity and magnetic susceptibility, a new method has been developed at ISU based on the tunnel diode oscillator (TDO) technique. The TDO technique uses the negative differential resistance of a tunnel diode to drive an LC tank circuit into self-sustained oscillation at the resonant LC frequency. The LC tank is inductively coupled to the samples under study, and changes in the electrical resistivity or magnetic susceptibility of the sample are manifested as changes in the resonant frequency. By measuring the frequency shifts of the TDO, insights can be made into changes in the materialu27s electrical and magnetic properties. This method has been validated by performing resistivity measurements on a sample of high purity Zr, and by performing measurements on the ferromagnetic transition in a low-carbon steel ball bearing. In addition to the development of the laboratory and its supporting instrumentation, an effort has been carried out to study the metastable phase formation in an Fe83B17 near eutectic alloy. Initial supercooling measurements using the ISU-ESL identified the formation of three metastable phases: a precipitate phase that shows stable coexistence with the deeply supercooled liquid, and two distinct bulk solidification phases. To identify the structure of the metastable phases, the Washington University Beamline ESL (WU-BESL) has been used to perform in-situ high energy x-ray diffraction measurements of the metastable phases. Based on the x-ray results, the precipitate phase has been identified as bcc-Fe, and the more commonly occurring bulk solidification product has been found to be a two-phase mixture of Fe23B6 plus fcc-Fe, which appears, upon cooling, to transform into a three phase mixture of Fe23B6, bcc-Fe, and an as-yet unidentified phase, with the transformation occurring at approximately the expected fcc-to-bcc transformation temperature of pure Fe. To further characterize the multi-phase metastable alloy, the ISU-ESL has been used to perform measurements of volume thermal expansion via the videographic technique, as well as RF susceptibility via the TDO technique. The results of the thermal expansion and susceptibility data have been found to be sensitive indicators of additional structural changes that may be occurring in the metastable solid at temperatures below 1000 K, and the susceptibility data has revealed that three distinct ferromagnetic phase transitions take place within the multi-phase mixture. Based on these results, it has been hypothesized that there may be an additional transformation taking place that leads to the formation of either bct- or o-Fe3B in addition to the Fe23B6 phase, although further work is required to test this hypothesis.
机译:爱荷华州立大学(ISU)已开发出一个新实验室,用于研究高温液体和固体,特别着重于液体及其亚稳态凝固产物的过冷。这个新实验室采用静电悬浮(ESL)技术,其中带电样品悬浮在一组电极之间,以实现非接触式处理。由于消除了坩埚,因此可以减少污染和异质成核的程度,从而实现样品的高温处理。由于异相形核的减少,样品可以在低于其平衡熔化温度的条件下进行过冷,从而为进行过冷液体的广泛测量打开了大门。已经实施了用于表征热物理性质的测量方法,例如:体积/密度,比热与总半球形发射率的比,表面张力,粘度,电阻率和磁化率。为了测量电阻率和磁化率,ISU开发了一种基于隧道二极管振荡器(TDO)技术的新方法。 TDO技术使用隧道二极管的负差分电阻来驱动LC谐振电路在谐振LC频率下进入自持振荡。 LC储罐与研究中的样品电感耦合,样品的电阻率或磁化率的变化表现为共振频率的变化。通过测量TDO的频移,可以洞悉材料的电和磁性能。通过对高纯度Zr样品进行电阻率测量以及对低碳钢球轴承中的铁磁跃迁进行测量,已验证了该方法的有效性。除了实验室及其支持仪器的发展之外,还努力研究了Fe83B17近共晶合金中的亚稳态相。使用ISU-ESL进行的初始过冷测量确定了三个亚稳相的形成:与深过冷液体稳定共存的沉淀相,以及两个不同的本体凝固相。为了确定亚稳相的结构,已使用华盛顿大学Beamline ESL(WU-BESL)对亚稳相进行原位高能X射线衍射测量。根据X射线结果,沉淀相被确定为bcc-Fe,并且发现更普遍的本体凝固产物是Fe23B6和fcc-Fe的两相混合物,冷却后,转化成Fe23B6,bcc-Fe和尚未鉴定的三相混合物,转化发生在大约纯Fe的预期fcc-bcc转化温度下。为了进一步表征多相亚稳态合金,已将ISU-ESL用于通过摄像技术测量体积热膨胀以及通过TDO技术进行射频磁化率的测量。已经发现,热膨胀和磁化率数据的结果是在低于1000 K的温度下亚稳固体中可能发生的其他结构变化的敏感指示,磁化率数据显示,在磁导率范围内发生了三个不同的铁磁相变。多相混合物。根据这些结果,可以推测,除了Fe23B6相以外,可能还会发生其他转化,导致bct-或邻-Fe3B的形成,尽管还需要进一步的工作来检验该假设。

著录项

  • 作者

    Rustan Gustav Errol;

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  • 年度 2014
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  • 原文格式 PDF
  • 正文语种 en
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