Table of Contents 1. Objective .................................................................... 2 2. Introduction ............................................................... 2 3. Experimental Work .................................................... 3 3.1 Equiment and Auxillaries: .................................. 3 3.

2 Experimental conditions: ................................... 3 3.3 Set up and Experimental Procedures: ................ 3 4. Results........................................................................ 4 5. Discussion .................................................................. 9 6. Questions ................................................................. 10

1. Objective
The main purpose of this experiment is to obtain the basic knowledge of SEM analysis. Characterize different samples and learn the impact on resolution, depth of field and different type of contrast when different electron accelerating voltages and working distances are applied.

2. Introduction
Since light-optical microscopy is limited by visible light (wavelength 400nm 700nm), the maximum resolution is about 200nm, the electron microscopy took its advantages in both high magnification and depth of focus. Scanning electron microscopy (SEM) is well performance on the material surface analysis. SEM device is briefly shown in the figure 1. It mainly consists of an electron emitting system, lens system, specimen chamber, and operating screen. The certain vacuum is needed in the whole device. An additional sample changing chamber is separated from the main chamber, providing a saving of time during changing samples.

Figure 1 construction of SEM In SEM, electrons are accelerated towards the surface of specimen. The interaction takes place between electrons and specimen, secondary electrons (SE) and back scattered electrons (BSE) are two important signal escaped from the surface, containing an energy ESE 50eV and EBSE 50eV. They are caught by detectors and then converted to image. In an electron gun, electrons are produced by thermal emission. The filament is heated up to operate the emission of free electrons. The accelerating voltage accelerates the electrons towards the anode. The impact of accelerating voltage is respectively important to the resolution of surface
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image, surface structure, edge effects and sample charge up. Working distance is the distance between sample and the final lens. It impacts the resolution of image and depth of field.

3. Experimental Work
3.1 Equiment and Auxillaries:
Smart SEM (Scanning Electron Microscope) (Brand: ZEISS Ultra Series Detection Plurality with Gemini Column.) Three samples for characterizing the structure and learning the influence\effect of variables like accelerating voltage, magnification and working distance etc. on the result and qualities of the micrograph. Sample 1: Gold coating on Si substrate Sample 2: ZnO (Zinc-oxide) coating on Si Substrate Sample 3: Sn (Tin) on carbon coated, coated with gold to increase conductivity and reduce the charge effect.

3.2 Experimental conditions:

Vacuum in the SEM column: 4.8x10-7 bar Vacuum in the filament\electron gun: 5.8x10-10 bar Others variables like magnification, working distance and acceleration voltage is mention below the micrographs.

3.3 Set up and Experimental Procedures:

3.3.1 Set up The SEM consists of a filament chamber where the electron source is produced. At least two pumps are needed in order to create a required vacuum inside it. The sample is placed into the specimen chamber through an exchange chamber without venting the whole system, as getting the vacuum is a long time procedure. In the control panel of the SEM the focus, magnification, contrast, brightness and stigmator correction buttons are found. The access to the digital imaging scanning system and the digital imaging processing system is made through the monitor of the computer placed aside the control panel. These programs are used to manipulate the image that one wants to get from the SEM.
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3.3.2 Experimental procedure The first thing to do is to install the sample in the chamber of the SEM; gloves must be worn so there is no contamination in the vacuum. For sample to be firm at their position, the sample must be screwed in a sample holder. Once the sample is ready, it is introduced in the exchange chamber, prior vent of it. After that, vacuum is applied in the exchange chamber so that the valve between the exchange and specimen chambers can be opened and the sample is transferred to the latter. After completing this procedure, the monitors are turned on. The high voltage is turned on, so it goes up until 12 kV. When the set-up of the SEM is done, Live SE is turned on in the Digital Imaging Scanning System to find the sample and focus it. Once the sample is found and focused, the magnification is increased in order to see the surface of the sample much clearer. With the Digital Imaging Processing System the photographs of the samples surface are saved and measures are taken, if necessary. The whole procedure is repeated for the remaining 2 samples. After the analysis of the samples, accelerating voltage put off. Finally, the sample is taken out and the exchange chamber has to be vented.

4. Results

Figure 1: Shows the surface micrograph of sample 1 at 917X Mag, 12KV Acc.
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volts and 2.6 WD.

Figure 2: Shows the micrograph of sample 1 (gold on Si substrate) at 2002X Mag, at same Acc. volts and WD as that of figure 1.

Figure 3: Shows the micrograph of sample 1 (gold on Si substrate) at much higher Mag 33470X.
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Figure 4: Shows the micrograph of sample 1 with astigmatism at 9320X.

Figure 5: Shows the micrograph of sample 1 without stigmatism at 9320X.

Figure 6: Shows the micrograph of sample-substrate-sample holder interface of sample 2 at 309X Mag for studying the density contrast effect in SEM micrographs.

Figure 7: Shows the microstructure of zinc oxide film (sample 2) at 3170X Mag and 12 KV Acc. Volts.
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Figure 8: Shows the microstructure of zinc oxide film on Si substrate (sample 2) at 3170X Mag and 1 KV Acc. Volts.

Figure 9: Shows the microstructure of sample 3 (tin on carbon) at 11130X Mag, 12 KV Acc. Volts and 2mm WD.

Figure 10: Shows the microstructure of sample 3 at 11150X Mag, 12 KV Acc. Volts and 9.2mm WD.

5. Discussion
Figure 1 to 5 correspond to the structure of thin film of gold (sample 1) at different magnification, the purpose behind that was to characterize the thin film of gold. Figure 1 reveals the network of gold (thin film) deposited on the silicon substrate, gold thin film has better contrast than silicon substrate which was looking as black in the background. At higher magnification Figure 2 shows that gold thin film (sample 1) composed of spherical, trigonal and hexagonal particles. At more higher magnification then 2000X it can be seen from figure 3 that the small spherical particles joined with the trigonal and hexagonal particles, aslo from figure 3 one can find the size of spherical particles which was approximately about 600 nm to 800 nm. Figure 4 show the presence of astigmatism which is basically the type of aberration in the objective lens, caused image stretching in one direction. It is very difficult to get information from such images because image was too blur, distorted and give false information as was stretched in one direction. Figure 5 has the same magnification as that of figure 4 but it without astigmatism. It is observed that the effect of astigmatism was more prominent at higher magnification. An image is said astigmatism free if it has no unidirectional defocussing when
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the objective lens was changed to under or over focus at a little high magnification. Figure 6 is the sample- substrate-sample holder interface, one can see the better contrast of ZnO than Si substrate and Aluminium sample holder, furthermore it was noted that Si substrate has better contrast the Al sample holder which was looking dark in the image. This effect is called Z contrast in SEM in which High Z (atomic number) material show better contrast than lower Z materials. The effect of accelerating potential can be observed by comparing figure 7 and 8 while keeping the magnification and working kept constant. Figure 7 contain high resolution, more edge effect and unclear surface structure where figure 8 contain less edge effects, low resolution but it contain clear surface structures. Moreover, it was concluded from both the micrograph that thin film of zinc oxide (sample 2) has a star like structure. The effect of working distance on the image can be seen clearly by comparing figure 9 and 10 while keeping magnification and acceleration potential keep constant. Higher working distance increased the resolution while the depth of field decreases, this can be seen by viewing figure 10 that contain high resolution while high depth of field obtain in figure 9. Moreover, figure 9 and 10 correspond to the sample which tin (Sn) coated on carbon, it was clear from the figure that the round particles were tin which were spread along the carbon matrix. Also high contrast of tin spherical particle then carbon matrix is because of Z contrast.

6. Questions
1. How can the range of usage of a light-optical microscope be extended? Resolution can be defined as the smallest distinct difference between two distinct points. Any resolution more this would be proved fruitless. The dependence of resolution can be found by Rayleigh rule; r = (0,61) / (sin) Higher resolution can be achieved by lowering the wavelength and decreasing the distance between the sample and the lens, as well as higher index of refraction. Changing of wavelength is near impossible in light microscope whereas increasing the lens magnification is also quite difficult. Hence only the distance between the objective lens and the sample can be decreased. 2. Which are the advantages/disadvantages of transmission electron microscopy (TEM) in comparison to scanning electron microscopy (SEM)? The advantages of TEM in comparison with SEM are; it has a higher
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resolution (as small as 0.2 nm) and that it shows a direct imaging of crystalline lattice and delineates defects (like dislocation, twin boundaries and tilt boundaries) inside the sample, while SEM shows only the surface of the sample. The disadvantage of TEM in comparison with SEM is that an electron-transparent sample is required and its preparation is difficult. 3. Which are the scattering types that can occur at atoms in case of accelerated electrons? Give some examples. Elastic or inelastic scattering can occur. In the case of the elastic scattering there is no significant energy loss, therefore the electron can leave the solid. One example would be the backscattered electrons, which are created by the interactions between electrons from the probe and atoms or between electrons from the probe and the crystal lattice. The inelastic scattering occurs when there are energy losses and the electron remains in the solid. Some examples are: Secondary electrons, X-rays, Auger electrons, formation of electron-hole pairs resulting in cathode-luminescence. These are created due to the transfer of energy from the primary electrons to the solid. 4. Field emission SEM: Describe the principle. Which are the advantages of this method? The principle of a Field Emission SEM (FESEM) is as follows. Electrons generated by a Field Emission Source (cold cathode field emitter) are accelerated in a field gradient under vacuum. The beam passes through electromagnetic lenses, focusing onto the specimen, so that different types of electrons are emitted from the sample. A detector gets the secondary electrons and an image of the sample surface is constructed by a comparison of the intensity of the secondary electrons to the scanning primary electron beam. The image is displayed in a monitor. The advantages of FESEM are: - It produces a clearer and less electrostatically distorted image with a spatial resolution lower than 1.5 nm (3-6 times better than regular SEM). - High quality, low voltage images are obtained with negligible electrical charging of samples.

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