High resolution SEM imaging of carbon nanotubes; deconvolution and retrieval of intrinsic nanotube dimensions
Characterizing physical properties of individual nanotubes is crucial for their implementation in nano electromechanical systems (NEMS). This requires measurements on suspended or free-standing structures together with accurate determination of the nanotubes dimensions. In situ methods are often used where physical measurements are performed inside electron microscopes [1-3]. Transmission electron microscopy (TEM) has the advantage of high resolution, providing accurate determination of both dimensions and the internal structure. The space inside a TEM is however rather restricted, leaving limited room for additional probes . Scanning electron microscopy (SEM) on the other hand, has a large specimen chamber which facilitates the addition of probes, but the image resolution is lower, making the evaluation of material properties less accurate or even impossible for very thin nanotubes . One way to solve this is to first measure the physical properties inside an SEM, and then determine the diameter using a TEM afterwards . This approach requires transfer of the nanotube from the SEM to a suitable TEM sample holder, and analysis of the same sample-location in both instruments. It would thereby be advantageous to obtain accurate structural information directly inside the SEM .
We have studied the mechanisms involved in SEM image formation of small multiwalled nanotubes, 2-5 nm in diameter. The electron-probe shape in an SEM broadens the sample details, and the image can be seen as a convolution of the secondary electron yield at each sample position and the probe shape. By comparing SEM and TEM images, we found that the probe intensity profile was best described by a linear combination of Gaussian and Lorentzian distributions. Using the obtained probe shape, the SEM images could then be deconvoluted to reveal more details, including the inner diameter in some cases. We also show how the outer diameter can be obtained by differentiating image profiles, a method that does not require any detailed knowledge regarding the probe shape and is reliable down to dimensions comparable to the electron-probe size. This significantly improves the capabilities of in-situ SEM experiments by enabling accurate characterizations of nanofibres inside SEM instruments, without the need for subsequent TEM imaging.
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