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Field Ion Microscopy for the Characterization of Scanning Probes

  • Chapter
Surface Science Tools for Nanomaterials Characterization

Abstract

Scanning probe microscopy (SPM) is a widely used tool for investigating the nanoscale structure of materials, as well as their electronic and mechanical properties with its related spectroscopic modes of operation. In SPM experiments, the sharp tip which probes the material under investigation is usually uncharacterized; however, its geometry and chemical composition play a large role in the SPM’s lateral imaging resolution and the features recorded in electronic and force spectroscopies. To carry out comparisons with modeling, one must consider a set of plausible tip structures and choose the one which best reproduces the experimental data recorded with the uncharacterized tip.

With an atomically defined tip prepared by FIM, the electronic and mechanical properties of the SPM probe are predetermined before the experiment, permitting direct comparison with theory, as well as the quantitative determination of parameters which depend on tip radius, such as stresses during indentation.

Here we describe the implementation of FIM for the characterization of scanning probe apices. This includes topics of tip integrity, characterization, advanced preparation methodologies, and key research findings from experiments which combine FIM and SPM techniques.

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Notes

  1. 1.

    We note that single-atom chemical sensitivity has also been achieved recently in STM and AFM techniques: inelastic electron tunneling spectroscopy in STM allows for measurement of the vibrational energies of individual chemical bonds, which is a form of chemical sensitivity – for example one can distinguish between hydrogen and deuterium bonds [18, 19]. In the case of AFM, however, it is more of a relative chemical sensitivity obtained by comparing force-distance interaction curves from different atomic species with the same tip. Absolute chemical identification relies on the specifics of the tip apex which is usually unknown [6].

  2. 2.

    An unconventional setup which allows tungsten probes, compatible with the high electric fields in FIM, to be used as SPM tips. The development of new AFM force sensors such as the qPlus [30] and length extension resonator [31, 32] conveniently allow tungsten probes to be used for AFM.

  3. 3.

    These fields are the highest achievable by laboratory techniques and are comparable in magnitude to those inside ionic crystals [10].

  4. 4.

    For example, the MCP is bombarded by 200 eV electrons for many days to remove gas atoms trapped in the channels.

  5. 5.

    Even in the case of admitting ultrapure He through a heated quartz tube, the normal pumping speed of the UHV system may have to be sacrificed during FIM. In our case, the turbo pump must be valved off as the heated quartz cannot provide a sufficient flux of He to reach 10−5 mbar.

  6. 6.

    A technique used by Müller with film and color photographic printing to identify individual changes among the many atomic sites on a FIM tip [81]. Here, it is done digitally.

  7. 7.

    FEM operates in a similar manner to FIM, but a field emission current is detected rather than field ionized gas atoms. A spatial map of the field emission current is visualized on an MCP/phosphor screen when the tip is negatively biased. The technique does not allow the atomic structure of the tip to be imaged.

  8. 8.

    Though the frequency of spikes was very much less on some of these substrates, their presence was still correlated with changes to the FIM tip.

  9. 9.

    If the latter were the case, tip changes would be seen all over the apex region from chemically bound atoms.

  10. 10.

    The images of modified tips that we display are taken at as low a voltage as possible to minimize tip changes, but it is impossible to determine how many atoms desorb before the onset of imaging. Numerous images are acquired while the voltage is slowly increased; they are averaged together in sets where the tip structure remains constant. The stability of modified tips may increase with decreasing temperature. However, changing the temperature will not change the ionization field of the adsorbed atoms relative to tungsten or the imaging gas.

  11. 11.

    It takes many layers of field evaporation to increase the radius significantly.

  12. 12.

    In order to screen for tip changes during the STM experiment itself, one may want to acquire a higher bandwidth version of the tunneling current signal throughout the entire experiment to scrutinize carefully for spikes. By higher bandwidth, we mean the several kHz bandwidth of the current preamplifier, rather than the ∼100 Hz pixel STM scan rate.

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Authors and Affiliations

  1. Physics Department, McGill University, 3600 University, Montréal, QC, Canada

    Peter Grütter

  2. IBM Research Division, Almaden Research Center, 650 Harry Road, San Jose, CA, 95120, USA

    William Paul

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  1. William Paul
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  2. Peter Grütter
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Correspondence to William Paul .

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  1. Center for Advanced Microstructures and Devices, Baton Rouge, LA, USA

    Challa S. S. R. Kumar

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Paul, W., Grütter, P. (2015). Field Ion Microscopy for the Characterization of Scanning Probes. In: Kumar, C.S.S.R. (eds) Surface Science Tools for Nanomaterials Characterization. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-662-44551-8_5

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