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Chapter 3 Scanning Electron Microscopy 255

Figure 3–68. ESBD patterns from an as-cast niobium specimen. (a) High-resolution EBSD pattern with

background subtraction. Exposure time, 7 s. (b) Raw data EBSD pattern for high-speed mapping.

Exposure time, 15 ms. EBSD patterns are recorded with thermal FESEM JSM-6500F. (c) EBSD pattern

from (a) with colored pairs of Kikuchi lines generated by automatic indexing. [EBSD patterns were

kindly provided by Dr. S. Zaefferer, Max-Planck-Institut für Eisenforschung, Düsseldorf, Germany. (a

and b) From Zaefferer, 2004; with kind permission from JEOL (Germany) GmbH, München, Germany.]

(For part c, see color plate.)

tion obtained amounts to about 50 nm (at E

= 15 keV), i.e., smaller

grains or precipitates cannot be detected in the orientation map. The

map shown in Figure 3–69c provides information about the grain

boundary character and the orientation variations inside of each grain.

The latter is shown for an individual grain in more detail in Figure

3–70.

The OIM developed into a powerful technique providing a wealth

of information about the type and distribution of different phases, the

size, shape, and defects of grains, the type of grain boundaries, the

local crystal orientation, and the preferential orientation (texture). To

take full advantage of this new imaging technique in terms of spatial

and orientation accuracy the thermal ﬁ eld emission SEM providing a

high beam current is most suitable. Furthermore, the SEM needs a very

high mechanical and electronic sta bility because EBSD measurements

require very long recording time, e.g., up to 12 h for very large orien-

tation maps (Zaefferer, 2004). Finally, the preparation of specimens is

a very delicate task since EBSD is a very surface-sensitive technique

with an information depth of less than 10 nm up to a few tens of nano-

meters. Thus, the surface-near zone must be free of any deformation

and, in addition, the surface has to be rather smooth because any

surface relief may affect data acquisition.

The application of OIM is not restricted to metals and alloys. Crystal-

line materials such as semiconductors (e.g., Wilkinson, 2000), cera mics

(e.g., Katrakova and Mucklich, 2002; Koblischka and Koblischka-

Veneva, 2003), and minerals (e.g., Mauler et al., 2001; Prior et al., 1999)

can be investigated.

256 R. Reichelt

5.00 µm = 100 steps

colour coding:

hatched areas:

austenite

111

001

b) c)

grain boundary character

rotation angle fraction

41˚ 42˚ 0.051

42˚ 43˚ 0.112

43˚ 44˚ 0.140

44˚ 45˚ 0.132

45˚ 46˚ 0.097

46˚ 47˚ 0.018

deviation to

centre grain

orientation

orientation class

<001> ll ND (max. 20˚)

all other orientations

austenite

101

Figure 3–69. Secondary electron micrograph of austenite (a) with rough (1), relatively smooth (2), and

smooth (3) surface areas. (b) Orientation map of (a) measured by automated crystal orientation

mapping and color coded for the crystal direction parallel to the normal direction (ND) of the sheet.

Hatched areas correspond to austenite grains. (c) The boundary character between γ- and α-grains,

different orientation components [(001)||ND, red; all others blue] and the orientation variations inside

of each grain (color shading; b, bainite). The micrograph and the maps are recorded with thermal

FESEM JSM-6500F. Note: the extension toward the top and bottom of the measured are in (b) and (c)

mission from Elsevier.) (For parts b and c, see color plate.)

Chapter 3 Scanning Electron Microscopy 257

Acknowledgments. I would like to acknowledge the very valuable help

of Dipl.-Ing. Harald Nüsse [Institut für Medizinische Physik und

Biophysik (IMPB)] in preparing numerous schematic drawings and

ﬁ gures composed of individual micrographs. Dr. Vladislav Krzyzanek

(IMPB) kindly contributed data from Monte Carlo simulations of the

electron scattering in thin and in bulky specimens. I am greatly

indebted to Mrs. Ulrike Keller (IMPB) for expert technical assistance

in the preparation and scanning electron microscopic investigation of

numerous specimens. Finally, the expert photographic work of Mrs.

Gudrun Kiefermann (IMPB) with those micrographs, which were

recorded in the Institut für Medizinische Physik und Biophysik, is

greatly acknowledged.

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