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Title: YiKoan Hong


1
Ch 3. Optical properties
2001. 4 . 16. Yi-Koan Hong Department of
Metallurgy and Materials Engineering Hanyang
University, Ansan, Korea
2
Outline
  • Introduction
  • - Optical and Electron Microscopy
  • i ) The Optical Microscope-resolving power
  • ii ) The Transmission Electron Microscope
  • iii ) The Scanning Electron Microscope
  • iv ) Dark - field Microscopy the
    ultramicroscope
  • - Light Scattering
  • i ) The Tyndall effect - turbidity
  • ii ) Measurement of scattered light
  • iii ) Light Scattering theory
  • iv) Dynamic light scattering

3
The Optical microscope resolving power
  • d ? / 2n sin a
  • ( a angular aperture, n refractive index, n
    sin a numerical aperture of the objective lens
    for a given immersion medium )
  • d K1? / NA ( for increased resolution Small
    ?, Large NA )
  • DOF K2? / NA2

Better resolution
Decreased DOF
4
The observation of particles located at a defined
level in the electrophoresis cell
5
The Electron Microscope vs Dark field Microscope
  • Two techniques for overcoming the limitations of
    optical microscopy are of particular value in the
    study of colloidal system
  • The Transmission Electron Microscope
  • The Scanning Electron Microscope

(The limit of resolution is greatly extended)
  • The Dark - field Microscopy

(The minimum observable contrast is greatly
reduced)
6
The Transmission Electron Microscope
  • To increase the resolving power of a microscope
    so that matter of colloidal dimensions may be
    observed directly, the wavelength of the
    radiation used must be reduced considerably below
    that of visible light.
  • Electron beams can be produced with wavelengths
    of the order of 0.01nm and focused by electric or
    magnetic fields.
  • The useful range of the TEM for particle size
    measurement is c.1nm-5µm diameter.
  • From the angle of shadowing and the length of
    shadows, a 3D picture of the specimen can be
    built up.
  • A most useful technique for examining surface
    structure is that of replication

7
The Transmission Electron Microscope
Fiq 3.1
Fiq 3.2
8
The Scanning Electron Microscope (I)
  • In the scanning electron microscope a fine beam
    of medium-energy electrons scans across the
    sample in a series of parallel tracks.
  • These interact with the sample to produce
    various signals.
  • - SEE (Secondary electron emission)
  • - BSE (Back-Scattered electrons)
  • In the SEE mode The particles appears to be
    diffusely illuminated, particle size can be
    measured and aggregation behavior can be studied,
    but there is little indication of height.
  • In the BSE mode The particles appears to be
    illuminated from a point source and resulting
    shadows lead to good impression of height.

9
The Scanning Electron Microscope (II)
  • The magnification achieved in a SEM(resolution
    limit of c.5nm) is less than in a TEM, but the
    major advantage of the technique(low numerical
    aperture) is the great DOF which can be achieved.
  • SEM can give a DOF several hundred times greater
    than that of the optical microscope.
  • In colloid and surface science this large DOF is
    extremely valuable in the study of the contours
    of solid surfaces and in the study of the
    particle shape and orientation.

10
The Dark - field Microscopy
  • Dark field illumination is a particularly
    useful technique for detecting the presence of,
    counting and investigating the motion of
    suspended colloidal particles.
  • The two principal techniques of dark-field
    illumination
  • - Slit
    - Cardioid
  • Dark-field methods do not help to improve the
    resolving power of a microscope and are,
    neverthless, an extremely useful for studying
    colloidal dispersions and sedimentation,
    electrophoretic mobility, the progress of
    particle aggregation, number-average particle
    size. Etc.

11
The Light scattering (I)
  • Light scattering result from the electric field
    associated with the incident light inducing
    periodic oscillations of the electron clouds of
    the atoms of the material in question these
    then act as secondary sources and radiate
    scattered light.

12
The Light scattering (II)
  • The Tyndall effect - turbidity The noticeable
    turbidity associated with many colloidal
    dispersions is a consequence of intense light
    scattering. For example, a beam of sunlight is
    often visible from the side because of light
    scattered by dust particles.
  • It/I0 exp-tl
    It I0 exp-tl
  • It the intensity of the transmitted light beam
    ,
  • I0 the intensity of the incident light
  • t turbidity,
  • lthe length of the sample

13
The Light scattering (III)
  • Measurement of scattering light
  • Intensity, polarisation and angular distribution
    of the light scattered from a colloidal system
    depend on the size and shape of the scattering
    particles, the interactions between them, and the
    difference between the refractive indices of the
    particles and the dispersion medium.
  • Light - scattering measurements are, therefore,
    of great value for estimating particle size,
    shape, and interactions, and have found wide
    application in the study of colloidal
    dispersions, association colloids.
  • Light scattering offers the advantage of
    particle size analysis

14
The Light scattering (IV)
  • Light Scattering theory

15
The Light scattering (V)
  • Scattering by small particles (by Rayleigh)
  • When electromagnetic wave of intensity I0 and
    wave-length ? falls on a small particles(ltc.
    ?/20) of polarisability a, oscillating dipoles
    are induced in the particles.
  • The particle then serves as a secondary source
    for the emission of scattered radiation of the
    same wavelength as the incident light.
  • Scattering by large particles ( by Debye and
    Mie)
  • The theory of light scattering is more
    complicated when one or more of particle
    dimensions exceeds c. ?/20. Such particles cannot
    be considered as point source of scattered light,
    destructive interference between scattered light
    waves originating from different locations on the
    same particle must be taken into account.

16
The Light scattering (VI)
  • Dynamic light scattering
  • The defined frequencies associated with laser
    sources makes it possible to exploit light
    scattering to study the motion of colloidal
    particles.
  • Light scattered by moving particle will
    experience a doppler shift to slightly higher or
    lower frequency depending on whether the particle
    is moving towards or away from the observer.
  • The measurement allows the diffusion coefficient
    of the particles to be calculated.

17
The Light scattering (VII)
  • Small angle neutron scattering
  • Neutron scattering is useful for the study of
    adsorbed material on hydrosol particles. the
    neutron scattering length densities of hydrogen
    and deutrium differ considerably.
  • By preparing a hydrosol in an appropriate H2O/D2O
    mixture, it is possible to match the neutron
    scattering length densities of the dispersion
    medium and the core particles.
  • The neutron beam thus sees only the adsorbed
    layer, the thickness of which can be estimated.
    Alternatively, the dispersion medium can be
    matched to the adsorbed layer to permit
    estimation of the core-particle size.
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