Contamination-Free TEM for High-Resolution Imaging of Soft Materials

2010 ◽  
Vol 18 (3) ◽  
pp. 32-35 ◽  
Author(s):  
Shin Horiuchi ◽  
Takeshi Hanada

Element-selective imaging and analysis at atomic resolution have become possible by the recent advancements in TEM and STEM. However, the spatial resolution in images of soft materials can be limited by electron beam damage and/or contamination. This contamination is a carbonaceous layer deposited on the specimen surface as a result of electron bombardment. Beam-induced specimen contamination is caused by polymerization of hydrocarbons that are present in a TEM specimen chamber. The electron beam reacts with stray hydrocarbons in the beam's path to create hydrocarbon ions, which then condense and form carbon-rich polymerized film on the area being irradiated. Figure 1a shows contamination spots created on a carbon thin foil by illuminating a beam with an intensity of 5.6 × 104 el/nm·s at an accelerating voltage of 200 kV. The thickness of the contamination spots can be estimated by electron energy-loss spectroscopy (EELS). With increase in the irradiation period, the intensity of the zero-loss peak decreases, but the overall intensities in the energy-loss regions of the spectrum increase (Figure 1b). The thickness (D) can be estimated using the equation, D = Λ·ln(It/I0), where Λ is the total mean free path for inelastic scattering, and It and I0 are the integral intensities of the overall spectrum and the zero-loss peak, respectively. Using this equation, the thickness of the contamination was found to be about 600 nm with a 10-minute irradiation.

Author(s):  
R. F. Egerton ◽  
S. C. Cheng

Electron energy-loss spectroscopy offers a rapid method of estimating the local thickness of a TEM specimen. The best-known procedure requires only measurement of the integrated intensity IO under the zero-loss peak and of the integral It under the whole spectrum (up to some suitable energy loss Δ). The thickness t is obtained from the formula:where λ(β) is the mean free path for inelastic scattering up to some angle β which is determined by the collection aperture (e.g. objective aperture in CTEM). In agreement with previous work we find that Eq. (1) is applicable over a wide range of thickness, typically 10-500 nm for EO = 100keV incident energy; see Fig. 1. Some deviation at large thickness might be expected as a result of the angular broadening produced by plural scattering, and because of contributions from electrons elastically scattered through angles greater than β.


Author(s):  
A. V. Crewe ◽  
M. Isaacson ◽  
D. Johnson

In order to determine the potential of electron energy loss Information as a contrast mechanism in transmission scanning microscopy, as well as to better understand the interaction of electrons with the specimen in any electron microscope, more knowledge is needed concerning the damage produced in the specimen by the beam. This is especially true in biological specimens where the radiation damage is very significant, but not well understood. To investigate this problem, we have begun a series of experiments studying the effects of the passage of a ∼20 kv electron beam through thin films of important biological molecules.


Author(s):  
L. Reimer ◽  
R. Oelgeklaus

Quantitative electron energy-loss spectroscopy (EELS) needs a correction for the limited collection aperture α and a deconvolution of recorded spectra for eliminating the influence of multiple inelastic scattering. Reversely, it is of interest to calculate the influence of multiple scattering on EELS. The distribution f(w,θ,z) of scattered electrons as a function of energy loss w, scattering angle θ and reduced specimen thickness z=t/Λ (Λ=total mean-free-path) can either be recorded by angular-resolved EELS or calculated by a convolution of a normalized single-scattering function ϕ(w,θ). For rotational symmetry in angle (amorphous or polycrystalline specimens) this can be realised by the following sequence of operations :(1)where the two-dimensional distribution in angle is reduced to a one-dimensional function by a projection P, T is a two-dimensional Fourier transform in angle θ and energy loss w and the exponent -1 indicates a deprojection and inverse Fourier transform, respectively.


Author(s):  
E. G. Rightor ◽  
G. P. Young

Investigation of neat polymers by TEM is often thwarted by their sensitivity to the incident electron beam, which also limits the usefulness of chemical and spectroscopic information available by electron energy loss spectroscopy (EELS) for these materials. However, parallel-detection EELS systems allow reduced radiation damage, due to their far greater efficiency, thereby promoting their use to obtain this information for polymers. This is evident in qualitative identification of beam sensitive components in polymer blends and detailed investigations of near-edge features of homopolymers.Spectra were obtained for a poly(bisphenol-A carbonate) (BPAC) blend containing poly(tetrafluoroethylene) (PTFE) using a parallel-EELS and a serial-EELS (Gatan 666, 607) for comparison. A series of homopolymers was also examined using parallel-EELS on a JEOL 2000FX TEM employing a LaB6 filament at 100 kV. Pure homopolymers were obtained from Scientific Polymer Products. The PTFE sample was commercial grade. Polymers were microtomed on a Reichert-Jung Ultracut E and placed on holey carbon grids.


2001 ◽  
Vol 7 (S2) ◽  
pp. 344-345
Author(s):  
G. Möbus ◽  
R.E. Dunin-Borkowski ◽  
C.J.D. Hethėrington ◽  
J.L. Hutchison

Introduction:Atomically resolved chemical analysis using techniques such as electron energy loss spectroscopy and annular dark field imaging relies on the ability to form a well-characterised sub-nm electron beam in a FEGTEM/STEM [1-2]. to understand EELS+EDX-signal formation upon propagation of a sub-nm beam through materials we first have to assess precisely the beam intensity distribution in vacuum and find conditions for the best obtainable resolution.Experimental Details:Modern TEM/STEM instruments combine features of both imaging and scanning technology. The beam forming capability approaches closely that for dedicated STEMs, while CCD recording devices allow us to measure the beam profile by direct imaging at magnifications up to 1.5 M. The recording of a “z-section” series through the 3D intensity distribution of the cross-over can therefore be realised by recording of a “condenser focal series”.


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