5.2 Work-Hardening and Recovery 189
emerging through surfaces can be marked by etching a cleavage or polished
surface as mentioned in Sect. 2.2. The etch pits can be observed by optical
microscopy up to a density of about 10
11
m
−2
. Replicas of smaller etch pits
produced by the heavy metal carbon shadowing technique can be observed
in the transmission electron microscope. This method allows one to count
representative values of intermediate dislocation densities up to 10
13
m
−2
.
Higher densities of dislocations are determined from diffraction contrast
TEM images of thin films of the deformed samples. From the total projected
length Λ imaged within the area A, the dislocation density is calculated by
=4Λ/(πAt) [328]. Here, t is the foil thickness, which can be determined from
the emergence points through both surfaces of a dislocation lying on a known
plane, or by other methods of diffraction contrast TEM. A simpler method
consists in superimposing a rectangular net of two sets of parallel straight lines
of nonconstant spacing onto the micrograph. The dislocation density is deter-
mined by counting the numbers of intersections N
1
and N
2
of the dislocations
along the two respective sets of grid lines. With the total lengths L
1
and L
2
of the grid lines, the dislocation density becomes =(N
1
/L
1
+ N
2
/L
2
) /t
[329]. If randomly oriented lines are used, the dislocation density is esti-
mated by =2N/(Lt) [330]. TEM extends the range of dislocation density
measurements up to about 10
16
m
−2
. It has to be considered, however, that
part of the dislocations may be invisible because of contrast extinction at the
particular imaging vector. Depending on the latter, in the f.c.c. lattice, the
fraction of the extinguished dislocations may amount up to 50%.
High dislocation densities can also be determined from the broadening
of X-ray diffraction profiles. A high sensitivity is necessary, which can be
achieved in the so-called self-focusing arrangement where the contribution
of the wavelength dispersion to the instrumental line-broadening disappears
[331]. The full width at half-maximum of the X-ray lines can be represented
by the modified Williamson–Hall plot [332] according to
ΔK ≈ 0.9/D +(π/2)
1/2
Mb
1/2
KC
1/2
+ higher terms in K
2
C,
where θ is the diffraction angle, λ the wavelength of the X-rays, K =2sinθ/λ,
and ΔK =2cosθ(Δθ)/λ. D is the particle or subgrain size, b is the magnitude
of the Burgers vector, and is the dislocation density. Furthermore, M is a
constant depending on the outer cut-off radius of the dislocations, and C is
the dislocation contrast factor, which depends on the relative orientations
between the Burgers and line vectors of the dislocations and the diffraction
vector as well as on the elastic constants. For cubic crystals, C values have been
calculated in [333]. The contributions to the line broadening from the particle
size and from the strains due to dislocations can be separated by plotting
ΔK vs. KC
1/2
. The method has been applied, for example, to determine the
gradients in the dislocation density between the bulk and surface regions of
deformed crystals.
The most sensitive and spatially resolving technique is the measurement
of the effective stress by using the dislocationsthemselvesasaprobe,thatis,