Films minces à base de Si nanostructuré pour des cellules ...
Films minces à base de Si nanostructuré pour des cellules ... Films minces à base de Si nanostructuré pour des cellules ...
ˆ The inuence of laser power density on the microstructure of the sample is investigated for possible laser annealing. 2.2.5 Electron Microscopy Microstructural analyses were done using High Resolution Transmission Electron Microscope (HR-TEM) and Energy-Filtered Transmission Electron Microscope (EF- TEM) 1 . The principle and working of these instruments are as detailed below and the schematic diagram is shown in gure 2.14. tel-00916300, version 1 - 10 Dec 2013 Figure 2.14: Schematic representation of light microscope, transmission electron microscope (TEM) and energy ltered TEM (EFTEM). High Resolution Transmission Electron Microscope Principle Transmission electron microscopy (TEM) technique is the most powerful one to investigate at the nanometer scale the structural properties of nanocrystals. It works on the same principle of a light microscope (optical microscope), the only dierence being the utilization of electrons instead of photons. TEMs use electrons as 'light source' and their much lower wavelength makes it possible to obtain resolutions that are a thousand times better than with a light microscope. 1 All the HRTEM observations were made by Prof X. Portier (CIMAP) and EFTEM observations by Dr. M. Carrada, CEMES, Toulouse, France. 46
Experimental set-up and working tel-00916300, version 1 - 10 Dec 2013 An electron beam, is produced by thermionic emission from a LaB 6 crystal or from a tungsten lament on application of current, and a potential dierence generated extracts the electrons. Electrons can also be produced using a eld emission gun with a tungsten tip when subjected to intense electric eld. This electron beam propagates in vacuum to illuminate the sample to be analyzed. In our laboratory JEOL 2010F set-up, the latter method is used. Instead of glass lenses focusing the light in the light microscope, the TEM uses electromagnetic lenses to focus the electrons into a very thin beam. The electron beam then interacts while travelling through the sample. Depending on the density of the material present, some of the electrons are scattered and disappear from the beam. At the bottom of the microscope the unscattered electrons hit a uorescent screen, which gives rise to a 'shadow image' of the sample with its dierent parts displayed in varied darkness according to their density. The image is then captured with a CCD camera for analysis. It is possible to observe either the image area exposed under the electron beam (image mode) or its associated diraction pattern (diraction mode). The diraction pattern also gives information on the orientation of the substrate during the observation. In Image mode, two types of contrast can be viewed. A diaphragm placed in the focal plane of the objective lens is used to select the electrons diracted in a particular direction and this image is called dark eld. The image from transmitted beam, is known as the bright eld image. Informations extracted in this thesis ˆ The crystallization and size of the Si-nps can be visualised. ˆ The total thickness of the sample, and individual sublayer thickness in a multilayer can be obtained. Energy Filtered Transmission Electron Microscope Principle Imaging Si nanoparticles in a SiO 2 (or Si 3 N 4 ) matrix by "traditional" TEM is not straightforward. Si nanocrystals exhibit only weak amplitude and phase contrast because of the small dierences in atomic number and density between Si and SiO 2 . For this reason, it is impossible to image individual Si-nps by conventional TEM (defocused bright eld or Fresnel contrast) as it is usually done for example for Ge-nps in SiO 2 . In the case of crystalline particles HR-TEM or dark eld (DF) imaging can 47
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Experimental set-up and working<br />
tel-00916300, version 1 - 10 Dec 2013<br />
An electron beam, is produced by thermionic emission from a LaB 6 crystal or from a<br />
tungsten lament on application of current, and a potential dierence generated extracts<br />
the electrons. Electrons can also be produced using a eld emission gun with<br />
a tungsten tip when subjected to intense electric eld. This electron beam propagates<br />
in vacuum to illuminate the sample to be analyzed. In our laboratory JEOL<br />
2010F set-up, the latter method is used. Instead of glass lenses focusing the light<br />
in the light microscope, the TEM uses electromagnetic lenses to focus the electrons<br />
into a very thin beam. The electron beam then interacts while travelling through<br />
the sample. Depending on the <strong>de</strong>nsity of the material present, some of the electrons<br />
are scattered and disappear from the beam. At the bottom of the microscope the<br />
unscattered electrons hit a uorescent screen, which gives rise to a 'shadow image'<br />
of the sample with its dierent parts displayed in varied darkness according to their<br />
<strong>de</strong>nsity. The image is then captured with a CCD camera for analysis. It is possible<br />
to observe either the image area exposed un<strong>de</strong>r the electron beam (image mo<strong>de</strong>)<br />
or its associated diraction pattern (diraction mo<strong>de</strong>). The diraction pattern also<br />
gives information on the orientation of the substrate during the observation. In<br />
Image mo<strong>de</strong>, two types of contrast can be viewed. A diaphragm placed in the focal<br />
plane of the objective lens is used to select the electrons diracted in a particular<br />
direction and this image is called dark eld. The image from transmitted beam, is<br />
known as the bright eld image.<br />
Informations extracted in this thesis<br />
ˆ The crystallization and size of the <strong>Si</strong>-nps can be visualised.<br />
ˆ The total thickness of the sample, and individual sublayer thickness in a multilayer<br />
can be obtained.<br />
Energy Filtered Transmission Electron Microscope<br />
Principle<br />
Imaging <strong>Si</strong> nanoparticles in a <strong>Si</strong>O 2 (or <strong>Si</strong> 3 N 4 ) matrix by "traditional" TEM is not<br />
straightforward. <strong>Si</strong> nanocrystals exhibit only weak amplitu<strong>de</strong> and phase contrast<br />
because of the small dierences in atomic number and <strong>de</strong>nsity between <strong>Si</strong> and <strong>Si</strong>O 2 .<br />
For this reason, it is impossible to image individual <strong>Si</strong>-nps by conventional TEM (<strong>de</strong>focused<br />
bright eld or Fresnel contrast) as it is usually done for example for Ge-nps<br />
in <strong>Si</strong>O 2 . In the case of crystalline particles HR-TEM or dark eld (DF) imaging can<br />
47