Dr. Saad B. H.

Farid

Electron Microscopy of Materials

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Electron Microscopy of Materials

Microstructural Analysis
Competition between Optical microscopy and Scanning Electron Microscopy SEM Optical Microscopy 800 1000, resolution 10 m Recent Laser Optical Microscopy, (405 nm Semiconductor Laser) The Confocal laser scanning microscope 17280, resolution 0.01 m

Optical Microscope

Scanning Laser Microscopy Advantages over SEM: 1. Sample preparation or microscope setup is unnecessary 2. Real-time observation 3. Observation can be made under atmospheric conditions 4. The measurement point is easily identified in the microscope. 5. Noncontact, nondestructive observation using a laser 6. Large samples can be accommodated making sample cleaving unnecessary 7. Line roughness and surface roughness analysis with Noncontact probing allows specimens to be free of scratches

Confocal Higher depth of field

Disadvantage: Limited Magnification and resolution compared with SEM

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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Scanning Electron Microscopy SEM

The electron source (or gun) is usually of the tungsten filament thermionic emission type, although field emission gun (FEG) sources are increasingly being used for higher resolution (Metal surface subjected to an extremely high electric field >109 V/m). The electrons are accelerated to energy which is usually between 1keV and 30keV which is considerably lower than the energies typical of the TEM (l00300keV). Two or three condenser lenses then demagnify the electron beam until, as it hits the specimen, it may have a diameter of only 210 nm.

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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All scanning electron microscopes normally have facilities for detecting secondary electrons and backscattered electrons. X-rays are used primarily for chemical analysis rather than imaging. Auger electrons are of such low energy, and are so easily absorbed that they require an ultra high vacuum system and specialized equipment for their efficient use. Auger spectroscopy and the scanning Auger microscope are important surface analytical techniques. Other signals are useful in applications that are more specialized.

Scintillator detectors These detectors are of the scintillator/light pipe/photomultiplier type, and are designed to maximize the solid angle of collection. Solid-state detectors When a high-energy electron impinges on a semiconductor, it produces many electronhole pairs, detected by the self-bias generated by a PN junction. Magnification: typically 20-106 Resolution: for modern systems, are typically - 3.0 nm at 30 kV (SE) - 4.0 nm at 30 kV (BSE) - 10.0 nm at 3 kV (SE) Depth of field Apart from its good spatial resolution, one of the most important aspects of the scanning electron microscope is its large depth of field, i.e. the resolution in the z-direction. Sample preparation for SEM exam For effective viewing of a specimen in the SEM, it is necessary for the surface of the specimen to be electrically conducting. This is to increase the electron yield, thus having adequate brightness.

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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Few nanometers coating with gold is a general experience to make the sample surface conductive. The examination of non-conducting specimens, particularly polymers and biological materials in the SEM may present other problems, such as specimen degradation by beam heating, radiation damage, and specimen volatility in the high vacuum. Thus, special techniques should be learned by the researcher/technician to overcome this difficulty. Applications of SEM (a Collection) 1. Observation of microstructure and topography

2. Observation of recrystallization, such as recrystallized twins in Cu-Sn (BSE image)

3. Test of welding cracks

SEI: topography contrast

BSEI: Z contrast

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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4. Distribution of e.g. Cu in welded steels (BSEI)

5. Element analyze and imaging (EDS)

6. Observation of multilayer binding (SEI, e.g. TiN-AlN on steel)

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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7. Analysis of fracture surface

Alumina, in-lens detector, 100 kX Brittle intergranular fracture Scanning Electron Microscope (SEM) image of intergrannular fracture indicative of hydrogen embrittlement. (Mag: 400X)

Ductile dimple fracture

Fatigue crack

Intragranular ductile failure

Transmission Electron Microscopy TEM

See figure next page. The SEM becomes a microprobe analyzer (EPMA) when an Xray detector is added, or a STEM when the detector is moved below the specimen. In a similar way an X-ray detector and/or an electron energy loss spectrometer (EELS) can he added to a TEM to make an analytical EM (AEM). Addition of scanning coils to this configuration results in a TEM/ STEM, while adding post-specimen lenses to a dedicated STEM at the other end of the diagram would achieve virtually the same configuration. The two ends of the Figure therefore effectively meet. Preparation of specimens for TEM A specimen must first be prepared before any observations can be made. It is not straightforward to make a specimen thin enough for TEM (a few tens of nanometers to a micron in thickness). The task is made harder still by the need to avoid changes in the specimen due to the preparation technique, and obtain a representative (or sometimes very specific) region. The sample must also be strong enough to handle, and last at least long enough to be examined in the microscope. These are tough requirements, and only rarely are

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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they all met. However it is worth striving for a specimen which gives the maximum amount of information with the minimum amount of complex interpretation, and this means that a great deal of emphasis should be placed on specimen preparation. The techniques employed vary greatly, depending upon the type of material being studied, and form the subject of several books and many scientific papers. The degree of difficulty in sample preparation can vary from being almost trivial to a skill which can take weeks to master. The different specimen preparation techniques can be divided into two basic approaches. First is removal of unwanted material, by either chemical or mechanical means, until only a very thin specimen is left behind. Second is cutting, in which the sample is either cut with a knife or cleaved along crystallographic planes so that a very thin specimen, or region of a specimen, is produced. We will describe here only the basics of the most commonly used techniques.

Figure: The family of electron microscopes. The two basic imaging systems (SEM and TEM) are shown in the centre. The addition of further detectors or lenses can give each microscope a range of analytical capabilities. X = X-ray detector; E electron detector. 1. Electro-polishing and chemical polishing The most common technique for thinning electrically conductive materials such as metals and alloys is electro-polishing. The principle of the method is that the specimen is made the anode in an electrolytic cell. When a current is passed, metal is dissolved from the anode (the specimen) and deposited on the cathode. The experimental arrangement can be very simple, as shown in Figure 4.39, or can be carried out in a sophisticated semi-automatic commercial unit but the principle is identical. If the composition of the electrolyte and the operating voltage are chosen successfully, a specimen in the form of a thin sheet not only becomes thinner hut also smoother. Eventually a hole appears in the thin sheet and if the neighboring regions arc sufficiently smooth (i.e. well polished), they will be thin enough for viewing in the TEM. The process is shown schematically in Figure 4.40. Cooling of the

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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electrolyte to low temperatures is often employed to change the kinetics of the etching process to produce a smooth surface. 2. Mechanical polishing Most materials science samples will he ground and/or polished as a first stage in the specimen preparation process. Grinding is usually done using paper which has a layer of hard particles, often SiC, stuck onto one face. The paper is graded according to the particle size, which can vary from a sizeable fraction of a millimeter to only a few microns. Usually the paper is placed on a wheel which spins while being lubricated by flowing water. The specimen is mounted on a jig, often using glue or thermoplastic wax, which allows the rate of removal of material to be controlled. The sample is initially ground flat using a coarse grit, and successively finer grits are used to remove the damage inflicted on the sample by the previous stage. Final polishing is often done using diamond powder a micron or less in size, either suspended in oil or water or embedded in a plastic film. Even finer polishing can be performed using mechano-chemical means, often using colloidal silica particles floating in an alkaline liquid.

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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Applications of SEM (a Collection) 1. Dislocation structure (diffraction contrast)

2. BF and DF images of dispersive precipitates in e.g. Al-Cr-Zr alloy

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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Bright Field BF

Dark Field DF

3. Observation of Organics

This meets versatile medical, biological pharmacological and other applications. 4. HR (high resolution) image of phase in Al alloys

Dr. Saad B. H. Farid

Electron Microscopy of Materials

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5. HR contrast image of metal atom arrangement in 1,97 nm thick specimen of Nb-W-O

GD Luck