Probing the Chemistry and Spectroscopy of Radiation-Sensitive Polymers by Parallel-Detection EELS

1990 ◽  
Vol 48 (2) ◽  
pp. 34-35
Author(s):  
E. G. Rightor ◽  
G. P. Young
Keyword(s):  
Electron Beam ◽  
Bisphenol A ◽  
Energy Loss ◽  
Parallel Detection ◽  
Commercial Grade ◽  
Incident Electron Beam ◽  
Ptfe Sample ◽  
Spectroscopic Information ◽  
Edge Features ◽  
Electron Energy Loss

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.

Parallel Detection of Electron Energy Loss Spectra in Direct Mode

1990 ◽  
Vol 48 (2) ◽  
pp. 82-83
Author(s):  
Eckhard Quandt ◽  
Stephan laBarré ◽  
Andreas Hartmann ◽  
Heinz Niedrig
Keyword(s):  
Energy Loss ◽  
Electron Energy ◽  
Energy Resolution ◽  
Large Angle ◽  
Maximum Energy ◽  
Semiconductor Detectors ◽  
Parallel Detection ◽  
Photodiode Arrays ◽  
Electron Energy Loss ◽  
Electron Energy Loss Spectra

Due to the development of semiconductor detectors with high spatial resolution -- e.g. charge coupled devices (CCDs) or photodiode arrays (PDAs) -- the parallel detection of electron energy loss spectra (EELS) has become an important alternative to serial registration. Using parallel detection for recording of energy spectroscopic large angle convergent beam patterns (LACBPs) special selected scattering vectors and small detection apertures lead to very low intensities. Therefore the very sensitive direct irradiation of a cooled linear PDA instead of the common combination of scintillator, fibre optic, and semiconductor has been investigated. In order to obtain a sufficient energy resolution the spectra are optionally magnified by a quadrupole-lens system.The detector used is a Hamamatsu S2304-512Q linear PDA with 512 diodes and removed quartz-glas window. The sensor size is 13 μm ∗ 2.5 mm with an element spacing of 25 μm. Along with the dispersion of 3.5 μm/eV at 40 keV the maximum energy resolution is limited to about 7 eV, so that a magnification system should be attached for experiments requiring a better resolution.

3d Reconstruction of Sub-Nm Beam Profiles in STEM

2001 ◽  
Vol 7 (S2) ◽  
pp. 344-345
Author(s):  
G. Möbus ◽  
R.E. Dunin-Borkowski ◽  
C.J.D. Hethėrington ◽  
J.L. Hutchison
Keyword(s):  
Electron Beam ◽  
Chemical Analysis ◽  
Energy Loss ◽  
Intensity Distribution ◽  
Dark Field ◽  
Beam Forming ◽  
Dark Field Imaging ◽  
Annular Dark Field ◽  
Electron Energy Loss ◽  
Field Imaging

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”.

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

2010 ◽  
Vol 18 (3) ◽  
pp. 32-35 ◽  
Author(s):  
Shin Horiuchi ◽  
Takeshi Hanada
Keyword(s):  
Electron Beam ◽  
Energy Loss ◽  
Thin Foil ◽  
Soft Materials ◽  
Mean Free Path ◽  
Loss Peak ◽  
Irradiation Period ◽  
Resolution Imaging ◽  
Electron Energy Loss ◽  
Beam Damage

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.

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