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    Resume Dry Practical 2

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    Dharmapadmi Kasilani
    The document summarizes scanning electron microscopy (SEM). It discusses the history and invention of SEM, how it works using electrons instead of light, its applications in observing surface topography, morphology, composition and crystal structure. It describes the instrumentation including the electron gun, lenses, detectors. It explains how SEM forms images through electron-sample interactions and the signals that can be used to characterize microstructure like backscattered electrons and X-rays. It also covers sample preparation and mounting, resolution, and the advantages of SEM over other microscopy techniques.

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    Resume Dry Practical 2

    Uploaded by

    Dharmapadmi Kasilani
    39 views6 pages
    The document summarizes scanning electron microscopy (SEM). It discusses the history and invention of SEM, how it works using electrons instead of light, its applications in observing surface topography, morphology, composition and crystal structure. It describes the instrumentation including the electron gun, lenses, detectors. It explains how SEM forms images through electron-sample interactions and the signals that can be used to characterize microstructure like backscattered electrons and X-rays. It also covers sample preparation and mounting, resolution, and the advantages of SEM over other microscopy techniques.

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    The document summarizes scanning electron microscopy (SEM). It discusses the history and invention of SEM, how it works using electrons instead of light, its applications in observing surface topography, morphology, composition and crystal structure. It describes the instrumentation including the electron gun, lenses, detectors. It explains how SEM forms images through electron-sample interactions and the signals that can be used to characterize microstructure like backscattered electrons and X-rays. It also covers sample preparation and mounting, resolution, and the advantages of SEM over other microscopy techniques.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    39 views6 pages

    Resume Dry Practical 2

    Uploaded by

    Dharmapadmi Kasilani
    The document summarizes scanning electron microscopy (SEM). It discusses the history and invention of SEM, how it works using electrons instead of light, its applications in observing surface topography, morphology, composition and crystal structure. It describes the instrumentation including the electron gun, lenses, detectors. It explains how SEM forms images through electron-sample interactions and the signals that can be used to characterize microstructure like backscattered electrons and X-rays. It also covers sample preparation and mounting, resolution, and the advantages of SEM over other microscopy techniques.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    of 6

    Dharmapadmi P. K.

    195160100111028

    Scanning Electron Microscopy (SEM)

    History of SEM
     In 1933, Electron Microscopy was invented by Ernst Ruska, a German
    physicist. He was a
     Awarded the Nobel Prize for physics for his invention in 1986
     In 1938, First SEM debuted by Manfred Von Ardenne
     In 1965, Cambridge Scientific Instrument (UK) and JOEL (Japan) first
    commercialized SEM individually

    Introduction of SEM
    The light microscope used photons while the electron microscope used
    electrons. Photons are substituted with electrons and glass lenses are
    substituted with electromagnetic and electrostatic lenses. The size of the light
    microscope is more than 100nm (the size of a Mycoplasma) and less than 1mm
    (the size of a frog egg). The size of an electron microscope is more than 0.1nm
    (the size of atoms) and less than 100µm (the size of eukaryotic cells). Electron
    microscopes are scientific instruments that use a beam of highly energetic
    electrons to examine objects on a very fine scale.

    Applications of SEM
     Topography is used to observe the surface features of the sample
     Morphology is used to observe the shape and size of the sample
     Composition is used to observe the elements that the sample is
    composed of and their relative amount (%) – purity
     Crystallographic info is used to observe how atoms are arranged in the
    sample
    The SEM image shows a more detailed picture of the object than the
    compound microscope image and TEM image. The TEM image shows a more
    detailed image of the object than the Compound microscope image.

    Instrumentation
    The parts of SEM include:
     Electron cannon
     Electron gun consisting of a cathode and anode
     The condenser lens controls the number of electrons traveling down the
    column
     The objective lens focuses the beam into a spot on the sample
     The deflection coil helps to deflect the electron beam
     SED attracts the secondary electrons
     Additional sensors detect backscattered electrons and x-rays
     Vacuum pumps system
     Operation panel with focus, alignment, and magnification tools and a
    joystick for positioning
     Screen for menu and image display
     Cryo-unit to prepare frozen material before insertion in the observation
    chamber in Cryo-SEM mode

    Formation of an image
    High-energy electrons shoot and the outgoing electron/x-rays analyze.
    SEM changes the magnification of an image by reducing the size of the area
    scanned by the scan coils. This form of image processing is only in gray. This
    image can be colorized through the use of feature-detection software. This is
    usually for aesthetic effects and adding a realistic effect.

    Electron beam-sample interactions


    The variety of products that are possible as a result of the interaction
    between electrons and matter can be seen. All these varied types of signals
    convey different beneficial information about the sample and it is the choice of
    the microscope’s operator which signal to capture. For instance, in
    transmission electron microscopy (TEM), as the name indicates, signals such
    as the transmitted electrons are detected which will provide information on the
    inner structure of the sample. In the case of a scanning electron microscope
    (SEM), two types of signal are usually detected; the backscattered electrons
    (BSE) and the secondary electron (SE).
    Parameters on Electron beam-sample interactions are the incident
    electron beam scattered in the sample, both elastically and inelastically. This
    gives rise to various signals that we can detect. Interaction volume increases
    with increasing acceleration voltage and decreases with increasing atomic
    number.

    Signals that can be used to characterize the microstructure


    Backscattered electrons (BSE) are a fraction of the incident electrons that
    are retarded by the electromagnetic field of the nucleus and if the scattering
    angle is greater than 180 ° the electron can escape from the surface.
    Backscattered electrons (BSE) consist of high-energy electrons originating in
    the electron beam, that are reflected or back-scattered out of the specimen
    interaction volume by elastic scattering interactions with specimen atoms.
    Heavy elements (high atomic number) backscatter electrons more strongly than
    light elements (low atomic number), and thus appear brighter in the image.
    One of the signals that can be used to characterize the microstructure is
    X-rays. Each element has a fingerprint X-ray signal. It has poorer spatial
    resolution than BSE and SE. Relatively few X-ray signals are emitted and the
    detector is inefficient (relatively long signal-collecting times are needed). The
    most common spectrometer is EDS (energy-dispersive spectrometer). Signal
    overlap can be a problem, so we can analyze our sample in different modes like
    spot analysis, line scan, and chemical concentration map (elemental mapping).
    Traditional guns or thermionic electron guns (electrons are emitted when
    a solid is heated) ( with W-wire, LaB6-crystal). Modern or field emission guns
    (FEG) (cold guns, a strong electric field is used to extract electrons) (with a
    Single crystal of W, etched to a thin tip). Usually, we want many electrons per
    time unit per area (high current density) and as small an electron spot as
    possible. By using field emission guns (FEG) we can get a smaller spot and
    higher current densities compared to thermionic guns, but we need a better
    vacuum for a FEG.
    There are 2 types of detectors, a Backscattered electron (BSE) detector
    (Solid-State Detector) and a Secondary electron (SE) detector (Everhart-
    Thornley). In traditional detectors. Traditional detectors, use those two
    detectors and Energy dispersive spectrometer (EDS) as the X-rays.
    The electron beam generated by the electron gun would encounter
    interference from air particles in the atmosphere. These particles block the
    path of the electron beam, they would also be knocked out of the air and onto
    the specimen, which would distort the surface of the specimen. Vacuum
    requirements are dependent on the type of detector. Chemical (corrosion) and
    thermal stability are necessary for a well-functioning filament (gun pressure).
    Charge-up is a phenomenon where the negative of the incident electron
    beam accumulates (charged up) on the surface of a non-conductive specimen
    and the potential in the beam-incident area changes to cause various image
    troubles. The charge-up phenomenon occurs when the total number of
    electrons emitted from a specimen, or backscattered electrons, absorbed
    electrons, and secondary electrons is not equal to the number of incident
    electrons. Charge-up can be prevented by coating the non-conductor sample
    with metal (conductor), allowing the charge on the sample surface to go to the
    ground through the coated conductive film.

    Energy Dispersive X-ray Microanalysis (EDX/EDS)


    An EDX spectrum was collected at each point identified in the top
    secondary electron image to individually characterize the wires. The resulting
    spectra show that the larger diameter wire is Ni, the medium diameter wire is
    Al, and the thinnest diameter wire is Ti. A small amount of Ai smeared onto the
    other wire surfaces when wires were wound together.

    Resolution
     Best resolution that can be obtained size of the electron spot on the
    surface of the sample
     The introduction of FEG has dramatically improved the resolution
    of SEMs
     The volume from which the signal electrons are formed defines the
    resolution
     SE image has a higher resolution than a BSE image
     Scanning speed :
     A weak signal requires slow speed to improve the signal-to-noise
    ratio
     When doing a slow scan drift in the electron beam can affect the
    accuracy of the analysis

    Sample preparation
    1. Coating specimen
    A coating specimen is used to increase the conductivity of the specimen
    and to prevent the high voltage charge on the specimen. All metals are
    conductive and require no preparation before being used. Meanwhile,
    non-metals need to be made conductive by using a device called a
    "sputter coater". These non-metals will coat with thin layers i.e. 20nm –
    30nm of conductive metal such as gold, gold-palladium alloy, platinum,
    osmium, iridium, tungsten, chromium, and graphite. Appropriate size
    sample that fits in the specimen chamber. Mounted rigidly on a
    specimen holder in specimen stub. For imaging in the SEM, specimens
    must be electrically conductive and electrically grounded.
    2. Cleaning the surface of the specimen
    Cleaning the specimen surface is very important because the surface
    contains a lot of unwanted deposits, such as dust, mud, soil, etc.
    3. Dehydrating the specimen
    Dehydration of the specimen using water must be removed, air drying
    causes collapse and shrinkage, this is usually achieved by replacing the
    water in the cell with an organic solvent such as ethanol or acetone,
    dehydration is carried out with a graded sequence of ethanol or acetone.
    4. Drying the specimen
    Dry the specimen by ensuring that the specimen is completely dry.
    Otherwise, the sample will be destroyed.
    5. Mounting the specimen
    Furthermore, the way to place the specimen is that the specimen must
    be mounted on a holder, rigidly mounted on specimen holder called a
    specimen stub. For dry specimens, it is attached to the specimen stub
    using an adhesive such as epoxy resin or electrically conductive double-
    sided adhesive tape.
    SEM Advantage
     Gives detailed 3D and topographical imaging and versatile information
    garnered from different detectors.
     Works very fast.
     Modern SEMs allow for the generation of data in digital form.
     Most SEM samples require minimal preparation actions.

    SEM Disadvantage
     SEMs are expensive and large.
     Special training is required to operate an SEM.
     The preparation of samples can result in artifacts.
     Limited to solid samples.
     Carry a small risk of radiation exposure associated with the electrons
    that scatter from beneath the sample surface.

    Environmental SEM (ESEM)


    Traditional SEM chamber pressure is about 10-6Torr while ESEM is
    0.08–30Torr. Various gases can be used by ESEM, and also requires different
    SE detectors. The reason for using ESEM is to image challenging samples such
    as insulating samples, vacuum (sensitive samples), irradiation (sensitive
    samples), and wet samples. Also, ESEM is to study and image chemical and
    physical processes in situ such as mechanical stress (testing), oxidation of
    metals, and hydration or dehydration.

    The use of FESEM in dentistry


    An example of the use of FESEM in dentistry can be used to look at a
    human tooth showing numerous dentin tubules X 900. It can be used to know
    the demineralization using etching with 37% phosphoric acid for 15 seconds
    and 10% sodium hypochlorite for 1 minute.
    Epitaxial growth such as enamel is made up of tightly bunched, oblong
    crystals that are about 1000 times smaller in width than human hair. Usually,
    we need more than one analysis/ data to better support our findings. Example:
    The use of various analyses in dentistry such as FESEM + XRD + HRTEM.
    The XRD Spectra indicated the evolution process from CPICs to HAP on
    the enamel window. SEM image showing both acid-etched enamel and repaired
    enamel. TEM image showing the longitudinal section of the reconstructed layer
    on natural enamel, including the native and repaired zone.
    It has been applied to research such as the Synthesis of ZnO using
    Bacillus cereus as the bio-templating agent (biomaterial as nanoreactor) and
    Zinc oxide synthesized using diethylene glycol-hydrothermal method showing
    carnation-like nanostructure.

    Summary
     SEM is a versatile instrument for many applications, especially for the
    study of surface morphology.
     To get a micrograph, an electron probe is scanned across the surface of
    the samples and detectors interpret the signal as a function of time
     A resolution of 1-2nm can be obtained when operated in a high-
    resolution setup.
     The introduction of ESEM and the field emission gun have simplified the
    imaging of challenging samples
     Signals:
     Secondary electrons (SE) are mainly topography
     Backscattered electrons (BSE) are mainly chemistry
     X-rays (EDX) is chemistry

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