Introduction To Microstructure
Introduction To Microstructure
Introduction To Microstructure
Practical 17 CP1
Course C: Microstructure
Introduction to microstructure
When describing the structure of a material, we make a clear distinction between its crystal
structure and its microstructure. The term ‘crystal structure’ is used to describe the average
positions of atoms within the unit cell, and is completely specified by the lattice type and
the fractional coordinates of the atoms (as determined, for example, by X-ray diffraction).
In other words, the crystal structure describes the appearance of the material on an atomic
(or Å) length scale. The term ‘microstructure’ is used to describe the appearance of the
material on the nm-cm length scale. A reasonable working definition of microstructure is:
In this course you will learn about how and why microstructures form, and how
microstructures are observed experimentally. Most importantly, microstructures affect the
physical properties and behaviour of a material, and we can tailor the microstructure of a
material to give it specific properties (this is the subject of the next course). The
microstructures of natural minerals provide information about their complex geological
history. Microstructure is a fundamental part of all materials and minerals science, and these
themes will be expanded on in subsequent courses.
This practical is in three parts. You should aim to spend a total of 60 minutes on parts 1 and
2, and 60 minutes on part 3.
ii. Some of the different processes that can lead to the formation of microstructures
iii. How we observe microstructures experimentally, and how the length scale of the
microstructure observed depends on the resolution of the experimental technique used
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Materials and Minerals Science
Practical 17 CP1
Course C: Microstructure
1.2 Phase/Component/Defect
A ‘phase’ is taken to be any part of a material with a distinct crystal structure and/or
chemical composition. Different phases in a material are separated from one another by
distinct boundaries.
A ‘defect’ is taken to mean any disruption to the perfect periodicity of the crystal structure.
This includes point defects such as vacancies and interstitials, planar defects such as
surfaces, twin boundaries, and grain boundaries, and as we will investigate in Course D,
dislocations.
You are provided with several photographs and hand specimens. In each case, write
down the number of components and phases present, and identify the types of defect
(if any) that are present. Make a labelled sketch of each one and add an appropriate
scale bar. The examples provided are:
Here we will examine some examples of microstructures formed by different processes. The
materials will be examined using both reflected-light and transmitted-light microscopes.
Ask your demonstrators for advice on setting up the two different types of microscope.
Guidelines are printed on separate sheets. Remember to look at the materials at a range of
magnifications: some microstructural details may only be visible at high magnification!
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Materials and Minerals Science
Practical 17 CP1
Course C: Microstructure
When a melt with limited miscibility between components solidifies, one often finds that
different phases solidify at different temperatures on cooling. In some cases, the different
phases form contemporaneously and become intimately intergrown with each other to form
complex (and often quite beautiful) microstructures. We will meet many examples of this
behaviour throughout this course.
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Materials and Minerals Science
Practical 17 CP1
Course C: Microstructure
Microscopy
You have met the principles of diffraction from lattice planes in Course A. Here we revise
some of the basic concepts and how they relate to the formation of images in a transmission
electron microscope (TEM). We will then use the laser benches to explore the resolution of
a system. The basic principles of image formation in a microscope (either an optical or an
electron microscope) are illustrated in Fig. 1.
u v
+θ
Incident beam of radiation
(light or electrons)
-θ
Radiation with wavelength λ is incident on the object (in this case a diffraction grating with
slit spacing d). Each slit in the grating scatters radiation in a variety of directions. Radiation
scattered in a given direction is collected by a lens placed at a distance u from the object and
focussed into a point in the back focal plane, located at a distance f from the lens. If the
condition dsinθ = nλ is satisfied (see Course A) then constructive interference occurs and a
bright diffraction spot will appear at that point. The image is formed at a distance v from the
lens. The image can be considered as the diffraction pattern of the diffraction pattern in the
back focal plane.
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Materials and Minerals Science
Practical 17 CP1
Course C: Microstructure
Transmitted light microscopes are set up on a side bench to examine diffraction gratings of
different spacings. When making these observations, it is important that none of the settings
of the microscopes are changed except as indicated below.
Three diffraction gratings are set in a single mount. Observe the grating with widest
spacing (100 lines/mm) taking care to focus precisely. Next look at the 300 lines/mm
grating and determine whether the lines are resolvable. (Any adjustment to the focus
should be extremely slight.)
With all the settings untouched, carefully remove the microscope eyepiece and look
down the tube with the eye several inches away from it. This gives a view of the back
focal plane of the microscope. Observe and sketch the diffraction pattern. Is your
observation consistent with that made when the eyepiece was in place?
With the eyepiece still removed, move the 100 lines/mm grating under the objective.
How many orders can be seen in the diffraction pattern? (Note: under some
circumstances this pattern can be difficult to see at first. It can help to move the eye
from side to side.)
Finally, observe both the diffraction pattern and the image of the fine grating (600
lines/mm). Are the lines resolvable, and could they be if the quality of the lens system
was improved?
From all your observations, estimate the resolution of the microscope as set up.
Compare this with the theoretical limit of resolution, dmin, for an optical microscope,
which is given by
λ
dmin ≈
n sin α
where λ is the wavelength of light (~0.5 µm), n is the refractive index of the medium
between the specimen and the objective lens (n ≈ 1 for air), and α is the acceptance
angle of the objective lens. The value of n sin α is usually printed on the side of each
lens as the numerical aperture, N. A.
Essentially the microscope is a tube whose diameter puts a maximum limit on the orders of
diffraction maxima which manage to exit the tube to form an image. Making the tube wider
increases the maximum resolution, but then the larger lenses suffer from more aberrations
which in turn need correction.
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Materials and Minerals Science
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Course C: Microstructure
Insert mask 12 (a zebra with unusually uniform stripes - see Fig. 2) in the holder in
front of the laser and set the screen of the optical bench at approximately 1 m from the
mask. Adjust the position of the lens (between 0 and 0.4 m from the mask) so as to
form a sharp image on the screen. Calculate the focal length of the lens.
(One or two sheets of paper under the lens mount will reduce the strength of the
magnetic clamping and make fine position adjustments easier.)
Replace the screen on the bench with the mirror provided, so that the beam is centred
on the second screen at the laser end of the bench (this is to increase the
magnification). Adjust the position of the lens so as to focus the zebra on the screen. It
will help to focus first on the edge of the zebra.
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Materials and Minerals Science
Practical 17 CP1
Course C: Microstructure
Briefly place the original screen in the back focal plane, which is one focal length
away from the lens, to observe the zebra’s diffraction pattern.
From your observations of the limits of resolution of an optical microscope, how could you
make the zebra lose its stripes?
Try out your solution (given the adjustable aperture provided – clue!). What is the
minimum amount of the diffraction pattern necessary to give the zebra a suggestion of
stripes? Draw a sketch of the ‘minimum pattern’.
Images formed from a single diffraction spot will not contain any information
about the periodicity of the object (i.e. its crystal structure), but they will contain
information about the general shape, size, and spatial distribution of phases and
defects in the object (i.e. its microstructure).
Images formed from all the diffraction spots are high resolution images which
allow us to visualise the periodicity of the underlying crystal structure.
On the next page are three images of the microstructure observed in a sample of the mineral
titanohematite (a solid solution containing hematite, Fe2O3, and ilmenite, FeTiO3). As this
mineral cooled very slowly over a period of 1 billion years, thin platelets (lamellae) of
ilmenite and hematite exsolved. Note that the length scale of the microstructure can vary
over several orders of magnitude within the same sample, with platelet widths varying from
mm to nm. This is caused by the gradual reduction in the distance over which atoms can
diffuse as the temperature decreases - platelets formed at high temperature are thick and
widely spaced, whereas those formed at low temperatures are thin and closely spaced.
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Materials and Minerals Science
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Course C: Microstructure
x22 1 mm x500 10 µm