Transmission Electron Microscopy Skills:Diffraction Contrast Imaging Lecture 10

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    (an embarrassingly short description ofan embarrassingly short description of )Diffraction Contrast Imagingiffraction Contrast ImagingLecture 10ecture 10

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    Categories of imagingategories of imagingMassass-thickness contrasthickness contrast Contrast appears in the image due to differences in the inherentontrast appears in the image due to differences in the inherent

    scattering from the samplecattering from the sample Z-contrast imaging (a highontrast imaging (a high-resolution version of same)esolution version of same)

    Diffraction contrastiffraction contrast In crystalline materials, diffraction occurs.n crystalline materials, diffraction occurs. Utilizing the objective aperture, either the direct (tilizing the objective aperture, either the direct (unn-diffractediffracted)beam or one of the diffract beams is selected to form the imageeam or one of the diffract beams is selected to form the image

    Results in crystallographic information being conveyed in the imesults in crystallographic information being conveyed in the imagegePhase contrast (hase contrast (highigh-resolutionesolution imaging)maging) Direct and diffracted beams undergo phase shifts in the materialirect and diffracted beams undergo phase shifts in the material An image if formed by recombining all beams and observing then image if formed by recombining all beams and observing the

    resulting interference patternesulting interference pattern

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    BF image formedfrom the direct beam

    Displaced apertureDF image formed

    with off-axis

    scattered beam

    CTF image where theincident beam is

    tilted so that the

    scattered beam

    remain on axis

    Bright Field / Dark Field Imagingright Field / Dark Field Imaging

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    Two beam imagingwo beam imaging

    Primary imaging mode is therimary imaging mode is the twowo-beameam conditiononditionAllows readily interpretable imagesllows readily interpretable images

    Bright Field Image Dark Field Image Weak-Beam DarkField Image

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    Twowo-beam conditionseam conditionsExamples of twoxamples of two-beameamconditions near the 011onditions near the 011Zone Axisone Axis

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    Twowo-beam conditionseam conditionsExamples of twoxamples of two-beameamconditions near the 011onditions near the 011Zone Axisone Axis

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    Kinematical Diffractioninematical DiffractionAssumptionsssumptions Only two diffracted beamsnly two diffracted beams

    considered, direct and oneonsidered, direct and onediffractediffracted Intensity of diffracted beam isntensity of diffracted beam issmallmall Single scattering eventingle scattering event Noo absorptionbsorption i.e.:.e.: IIdiffractediffracted

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    Kinematicinematic vs. Dynamicals. DynamicalCan be used to explain (to first approximation) the originan be used to explain (to first approximation) the originmuch of much what we see in the microscopeuch of much what we see in the microscopeHowever, cannot be used to accurately calculateowever, cannot be used to accurately calculateintensity relationshipsntensity relationshipsUse dynamical theory:se dynamical theory: Considers multiple beamsonsiders multiple beams Intensity in one or more diffracted beams can be large inntensity in one or more diffracted beams can be large incomparison with transmitted beamomparison with transmitted beam Multiple scattering allowedultiple scattering allowed Absorptionbsorption (loss of electrons) allowedloss of electrons) allowed Can explain intensity accuratelyan explain intensity accurately Very complicated to utilize practicallyery complicated to utilize practically

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    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystalsThickness contours:hickness contours: At exact Bragg condition (s = 0),

    the intensity of the direct anddiffracted beam oscillate in acomplementary way.

    For a wedge specimen, theseparation of the fringes in the

    image is determined by the angle

    of the wedge and the extinction

    distance, g.

    Thus, the image may appear to

    be black or white depending on

    the thickness of the specimenwhere you are observing it

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    111111

    hole

    aa

    Representative bright field (a),

    and dark field (b) micrograph

    showing thickness fringes

    100 nm100 nm

    bb 111111

    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystalsThickness contours:hickness contours: At exact Bragg condition (s = 0),

    the intensity of the direct anddiffracted beam oscillate in acomplementary way.

    For a wedge specimen, the

    separation of the fringes in the

    image is determined by the angle

    of the wedge and the extinction

    distance, g.

    Thus, the image may appear to

    be black or white depending on

    the thickness of the specimenwhere you are observing it

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    111111

    hole

    aa

    Representative bright field (a),

    and dark field (b) micrograph

    showing thickness fringes

    100 nm100 nm

    bb 111111

    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    Translation / rotationranslation / rotationbetween two crystalsetween two crystalsyields fringes in imagesields fringes in images Stacking faultstacking faults Grain boundariesrain boundaries Translation boundariesranslation boundaries Phase boundarieshase boundaries Surfaces (if stepped)urfaces (if stepped)

    Electron wave has alectron wave has adifferent amplitude &ifferent amplitude &phase in each crystalhase in each crystal Results in a fringe patternesults in a fringe pattern

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystals

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    gR causes the contrast and fordislocations, R changes with z.g

    b = n; if we know g and we determine n,then we know b.

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystalsStrain field of dislocation causes localdiffraction differencesSeen as line of contrast in the image (iforiented correctly )

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    0.5 m

    If gb = 0, then you wont see any contrast because the diffracting

    planes are then parallel to R.

    This is termed the invisibility criterion.

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    Weak-beam dark-field imaging

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    0.5 m

    If gb = 0, then you wont see any contrast because the diffracting

    planes are then parallel to R.

    This is termed the invisibility criterion.

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    0.5 m

    If gb = 0, then you wont see any contrast because the diffracting

    planes are then parallel to R.

    This is termed the invisibility criterion.

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    gR causes the contrast and fordislocations, R changes with z.g

    b = n; if we know g and we determine n,then we know b.

    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystalsStrain field of dislocation causes localdiffraction differencesSeen as line of contrast in the image (iforiented correctly )

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    100 nm100 nm100 nm100 nm

    001Al

    110 Al

    001001AlAl

    110110 AlAl

    Dark field images of new Al-2at.%Cu-1at.%Si-1 at.%Ge alloy aged 1h and 3hrs

    (right) at 190oC; imaged using 112 reflection.

    1h1h 3h3h

    Dark-field imaging

    Courtesy V.R. Radmilovic

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    Diffraction condition

    g

    2

    = t

    g

    2

    sin2(tseff )

    tseff( )2

    seff = s2 + 1

    g2

    eff = g

    w2 + 1

    Weak-beam dark-field imaging

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    Weak-beam dark-field imaging

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    Kinematicinematic diffraction in imperfectiffraction in imperfectcrystalsrystals

    Bright field image Dark field image

    Al2O3

    GaN

    Weak beamdark field image

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    111111

    hole

    aa

    Representative bright field (a),

    and dark field (b) micrograph

    showing thickness fringes

    100 nm100 nm

    bb 111111

    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystals

    Courtesy V.R. Radmilovic

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    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystals

    Bend Contours

    The origin of bend contours shown for

    a foil symmetrically bent on either side

    of the Bragg conditions. When thehkl

    planes are in the Bragg condition, the

    reflection G is excited.

    Bend ContoursBend Contours

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    [100]

    crystal

    orientationEach diffracted

    plane producestwo bend

    contours

    Kinematicinematic diffraction in perfectiffraction in perfectcrystalsrystalsBend ContoursBend Contours

    [103]

    crystal

    orientation

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    Categories of imagingategories of imagingMassass-thickness contrasthickness contrast Contrast appears in the image due to differences in the inherentontrast appears in the image due to differences in the inherentscattering from the samplecattering from the sample Z-contrast imaging (a highontrast imaging (a high-resolution version of same)esolution version of same)

    Diffraction contrastiffraction contrast In crystalline materials, diffraction occurs.n crystalline materials, diffraction occurs. Utilizing the objective aperture, either the direct (tilizing the objective aperture, either the direct (unn-diffractediffracted)beam or one of the diffract beams is selected to form the imageeam or one of the diffract beams is selected to form the image

    Results in crystallographic information being conveyed in the imesults in crystallographic information being conveyed in the imagegePhase contrast (hase contrast (highigh-resolutionesolution imaging)maging) Direct and diffracted beams undergo phase shifts in the materialirect and diffracted beams undergo phase shifts in the material An image if formed by recombining all beams and observing then image if formed by recombining all beams and observing the

    resulting interference patternesulting interference pattern