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Printed in Great Britain. All rights reserved Copyright c 1984 Pergamon Press Ltd
OVERVIEW NO. 37
E. HORNBOGEN
Institut fiir Werkstoffe, Ruhr-Universitlt, Bochum, F.R.G
Abstract-The structural level of “microstructure” is situated between that of “phase” and macroscopic
structures. An attempt is made at its complete and quantitative description. 0- to 3-dimensional defects
are classified as four groups of microstructural elements. These elements occur in different densities and
distributions. They can form order, mixtures, or gradients. Three elementary types of two-phase
microstructures (dispersion, net, duplex) are defined using as topological parameters densities of grain-
and phase-boundaries or the percolation behaviour of the phases and boundaries. These can be extended
to n-phase microstructures for which (n + 1) types exist. Complex microstructures contain mixtures of
elements and types. By analogy with transformations in other structural levels (electronic-. phase-) the
existence of microstructural transformations has been proposed. There are transformations of one
microstructural element into another (dislocations+ grain boundary), of defect crystals (microstructure)
into a glass phase (without microstructure), or of one two-phase microstructure into another type. Such
a microstructural transformation can be associated with large changes in bulk properties.
R&mm&-Le niveau structural de la “microstructure” est situ6 entre les niveaux des structures de “phases”
et des structures macroscopiques. Nous avons essaye d’en donner une description complete et quantitative.
Nous rangeons les defauts de dimension 0 a 3 en quatre groupes d’eliments microstructuraux. Ces
elements apparaissent avec des densites et des repartitions differentes. IIs peuvent former de l’ordre, des
melanges ou des gradients. Nous definissons trois types tlimentaires de microstructures diphasies
(repartition, r&au, duplex) en utilisant comme paramttres topologiques les densites des joints de grains
et de phases ou la percolation de ces phases et joints. On peut les etendre aux microstructures de n phases,
pour lesquelles il existe (n + I) types. Les microstructures complexes comprennent des melanges d’elements
et de types. Par analogie avec les transformations a d’autres niveaux structuraux (structure Clectronique,
phases), nous proposons l’existence de transormations microstructurales. II s’agit de transformations d’un
&l&rent microstructural en un autre (dislocations-+ joint de grains), de cristaux fautes (microstructure)
en une phase vitreuse (sans microstructure) ou dune microstructure diphaste en une d’un autre type. Des
changements importants de-s proprittes du mat&au massif peuvent itre associes a telle transformation
microstructurale.
ZtWUllUleQf-Die strukturelle Ebene “Gefiige” liegt zwischen der “Phase” und den makro-
skopischen Strukturen. Es wird ein Versuch zu dessen umfassender, d. h. vollstlndigen und quantitativen
Beschreibung gemacht. 0- bis 3dimensionale Gitterstiirungen werden als vier Grnppen von Gefiigeele-
menten festgelegt. Diese Elemente kommen in verschiedenen Dichten und Verteilungen vor. Sie kiinnen
Ordnung, Gradienten oder Gem&he bilden. Drei elementare Typen zwei-phasiger Gefiige (Dispersion,
Netz, Duplex) konnen mit Hilfe der Dichten von Kom- und Phasengrenzen als topologischer Parameter
definiert werden oder durch das Perkolationsverhalten (Durchdringung) der einzelnen Phasen. En-
tsprechend den Umwandlungen in anderen Ebenen der Struktur (elektronische Umwandlung, Phasen-
umwandlung) wird der Begriff einer Gefiigeumwandlung vorgeschlagen. Dies sind Umwandlungen eines
Geftigeelementes in ein anderes (Versetzung-rKomgrenze), eines defekten Kristalls (Gefiige) in eine
Glas-Phase oder eines zweiphasen Gefiiges in einen anderen Typ. Derartige Gefiigeumwandlungen konnen
mit grogen binderungen der makroskopischen Eigenschaften verbunden sein.
A 3 Atom w
N 2 Nucleus !-I
E , Elementary n
particle
I I I I I I 1 )
Level of IO-‘5 10-Q 10-q 10-6 10-x I00 I03
structure Size of structural objects (ml
The term microstructure is still often reserved to interface should be regarded as part of the micro-
objects which are visible by the methods of light structure, inspite of the fact that bi-crystal plus
microscopy. Its quantitative description has achieved interface may form a minimum free-energy system.
a high degree of perfection [ I.& Advances of electron Microstructure is identical with the arrangement in
microscopy (TEM, SEMI [3] and more recently field three-dimensional space of all types of non-
ion microscopy (FIM), however, have expanded our equilibrium defects including interfaces, and pores.
horizon so that it seems on time to extend the Thus a mono-phase alloy can, a poly-phase alloy
definition of microstructure. and to realise that its must have a microstructure.
importance is comparable to that of other levels of
structure.
The objects of concern in the different structural
levels cover a certain size range with considerable
overlap. The dimensions of microstructural elements
start just above one atomic spacing (as for example
the thickness of a grain boundary). The size of an
elementary cell of a crystal structure may surpass this
dimension by an order of magnitude (Fig. 1). Thus
the size cannot be used for a definition of the limit
between phase and microstructure. Phases are the
three-dimensional zones of homogeneous structure
(crystal or glass) and composition. Microstructure
comprehends all discontinuities inside and between
phases. The phases can be derived in most cases from
stable or metastable thermo-dynamical equilibria.
The elements of microstructure are non-equilibrium
features of structures. This allows a definition of the
limit between “phase” and “microstructure” [4],
which shall be discussed using the following exam-
ples.
The anti-phase domain boundaries (APB) in AuCu
are regularly spaced and required to minimize free
energy. They are considered if the elementary cell is
established and therefore part of the phase. At the
other hand, grown-in APB’s in FeAl do form an
APB-microstructure. They are not in equilibrium and
prone to healing out (Fig. 2). According to this
definition defects are regarded as part of the
microsrructure [S] unless they are required to min- Fig. 2. Distinction of phase and microstructure. (a) Antl-
imize the energy term of the free energy. Another phase domain boundaries (APB) belonging to the phase
limiting case is an interface of a bi-crystal. This AuCu. (b) Grown-in APB-microstructure in Fe,AI.
HORNBOGEN: ON THE MICROSTRUCTURE OF ALLOYS 617
(3d)
PZI = 0. (3e)
In a dispersion of p the matric 2 percolates the
cross-section of a macroscopic specimen. The same
Fig. 3. Examples for microstructureal elements: dis-
does fi for net structure (Fig. 5). For a similar
locations, stacking faults. grain boundaries in z-Cu + parameter the term contiguity was introduced
11.2 at.?, Ga solid solution. earlier [6.7].
.:
618 HORNBOGEN: ON THE MICROSTRUCTURE OF ALLOYS
ri!J
two-phase grain structures is the use of boundary
junctions (aaa, aa/& a/?/?, /?/IF) [9], and the densities of
boundary junction lines [equations (lb), (2b)] (Fig.
6).
Coating
3. MIXTURES OF MICROSTRUCTURAL
ELEMENTS AND TYPES
Dispersion
AU, provides the driving force for some solid state
Duplex Sceleton
reactions [lo]. Its amount characterizes micro-
Type of mlcrostructure
structural instability [ 141, provided that the structure
Fig. 4. Varieties of two-phase microstructures. is made-up of thermo-dynamically stable phases 4:
AF4 = 0.
The third type of two-phase microstructure is
AF,,,, = AF, + AF, (5b)
characterized by percolation of z as well as p, i.e. an
equal number of grains of equal average size is Thus characteristic for the structural level of micro-
arranged as a random mixture (Figs 5 and 6). Both structure is absence of thermo-dynamical equi-
types of grain boundaries. and interfaces occur with librium. Therefore a multititude of ways exist to
the same probability. In average seven interfaces and provide the energy for the formation of micro-
seven grain boundaries of both types touch each structure elements. For example the origin of two-
grain phase structures can be subdivided into the following
(Fig. 7):
PII = P/l/i @a)
(1) homogeneously nucleated (statistical distribu-
Pm + Pss = Pm/l (4b)
tion),
&p”B=!i?9=2 (2) heterogeneously nucleated (defect-controlled
w
Pm Pss . distribution),
(3) dissipative by autocatalytic growth (eutectic,
This is valid for the ideal duplex structure, which in
eutectoid growth),
addition requires a fixed ratio of the volume fractions
(4) synthetic (composites, sintered mixtures of
of the phases
different powders, structures formed by localized or
f, =fa = 0.5. W) periodic vapour deposition from different sources).
The average grain size of such a duplex structure S,, In this connection the origin of microstructural
is inverse proportional to the sum of the densities of order should be mentioned. Its occurrence is associ-
all boundaries [equation (2c)] ated with diffraction effects (side-bands) [l l-131. It
can be characterized by a decrease in microstructural
s,-Ph’=(P..+PBB+P.B)-‘. (k) entropy AS, as compared to the corresponding ran-
Each tl- or p-grain is surrounded in average by 14 dom microstructure (Fig. 8). Microstructural order
neighbours. The chance that they are all unlike is can be due to:
2-14. From this follows percolation of z and fi in the
(A) minimation of energy (AUr+min),
duplex structure (Table 3).
(B) dissipative growth,
tFor all microstructural elements (Table 1) (except for (C) artificial production.
thermal vacancies) the energy term AU, dominates and
entropy AS, can be neglected. This is also true for
Order is either controlled by thermo-dynamical equi-
entropy changes which occur as a consequence of librium (A) 1121, or kinetics of irreversible processes
microstructural order and disorder. (B), or human intelligence (C) [13].
HORNBOGEN: ON THE MlCROSTRUCTURE OF ALLOYS
Fig. 7. Different origin of two-phase microstructures. (a) Homogeneously nucleated: Fe + 1.1 at.“,, Cu,
25h 500’C. (b) Heterogeneously nucleated at dislocations: Fe + 1.1 at.“,;Au, 24h 500-C. IOh 550 C.
(c) Formed by autocatalytic reaction (combined discontinuous precipitation and recrystallization):
Cu + 2.8 at.%Co. 10% C.W. (d) Artificial formation by impregnation: Metglass, Fe + 20 at.!, B, in
epoxy-resin, fracture surface.
structural elements for example interact with mobile occur in all levels of structure (Fig. 1). Nuclear and
dislocations. They become elementary hardening electronic transformations are known as well as phase
mechanisms, and the yield stress of an alloy can be transformations in solids: a crystal structure z trans-
obtained even for a complex microstructure [16] forms into /I
(Table 1).
&+&I. (7a)
4. MICROSTRUCTURAL TRANSFORMATION Transformations paramagnetic-+ferromagnetic, or
Transformation is a (discontinuous or continuous) normal conductor-+superconductor are electronic
change in structure of matter. Transformations can transformations, the changes in phase structure are
Fig. 8. Microstructural order. (a) Ordered local distribution of particles, schematic. (b) Fe + 28 at.g;Ni t
R at.%Al, 1500h 4OWC,7 + ;t’.
HORNBOGEN: ON THE MICROSTRUCTURE OF ALLOYS 621
bcohrren,-‘b,m,.,oherml~bn,,-
crcn, (7d)
(4, + w 4, (8a)
The density of microstructural elements p, can attain
an upper limit. If. for example. the dislocation density
pd [equation (lb)]. or the boundary density oh (equa-
tion (1b)] reaches a value at which the spacing S,
[equation (2)] approaches atomic dimensions. an
amorphous phase is obtained (at about S,,, = 20 ).
Before this transformation is acquired an ultra-fine
crystalline microstructure exists. This transformation
is driven by external energies. For example dis-
locations are produced at surfaces exposed to fric-
tional shear stresses. Such high dislocation densities
must be stabilized by a sufficient number of inter-
stitial atoms such as B. C. N in r-iron (Fig. 13) [20].
If the density of grain boundaries is increased to a
spacing of S, < 10a. the volume fraction of the
(a)
“’ -A/ *
t
Nucleotlonof dlslocatlons
anneollng tune (I I
(C) Transfomations between d@rent types of micro - boundary densities have to be used to define certain
structure types of structures [equations (3), (4), (9)]. A trans-
These are defined by appearence of new micro- formation of one type of microstructure to another is
structural elements as topological parameters. They associated with the appearance or disappearance of a
should not be confused with a topological trans- particular type of boundary (Table 2, Fig. 15). which
formation of a geometrical structure by which topo- acts as a topological feature. Transformations can
logical features are preserved (Fig. 1I). Two-phase take place as a function of volume fraction of the
microstructures shall serve as examples for such phases, and of their shape and orientation. For
transformations. In addition to volume fraction, constant shape- and size-distribution the trans-
(0) lRD/PS
,
Crystok with
mlcrOSlrUCtUre
/’
P--P
(, b mm 0
*RN s,= 26
Density of grotn
boundones, p,,” She’
(b)r.. ‘.:
Fig. 14. Volume fractions of crystal and boundary and glass
transformation, schematic.
(a)
(b)
fz05 f < f, = k6
Fig. 1.5.Transformations of type of microstructure in planar sections schematic. (a) Dispersion@net. (b)
Duplex%dispersion.
5. CONCLUSIONS
A concept of microstructure useful for materials
science should fulfil the following requirements: it
a
- ‘6
h
C Insulator S Conductor
.>
t
z
::
bulk properties
p, ‘P, (14a)
PI = pp. U4b)
supplementary aspects for a complete description of 14. J. M. Martin and R. D. Doherty, Sfabiliry qf Micro-
microstru~u~ (the term morphology is used for strurture in MezaI~ic Systems. Cambridge Univ. Press
these materials). The concepts of microstructure will ( 1976).
15. E. Hombogen, Z. Mefallk. 64, 867 (1973).
also have to be supplemented for concrete. In addi- 16. E. Hombogen, Proc. ICSMR 5, Aachen. 2, 1337
tion to pores and fissures, structural gradients in (1979).
the cement phase play an important role [24]. A 17. Phase Transformations Am. Sot. Metals, Metals Park,
unified definition of microstructure which includes OH (1970).
18. Marrensitic Transformation. Proc. lnl. Summer Course
these two important classes of materials will still
(edited by L. Delaey). Leuven, BeIgium (1982).
require considerable efforts. 19. E. Hombopen, Z. .&feral/k. 72, 739 (1981).
20. E. Hombogen. K. H. Klein and J. Schmidt, J. Mater,
Sci. L.err. 1, 94 (1982).
21. H. Gleiter, in Polycrystals. Prvc. ad Rise Inr. Symp.
Acknon$edgemenrs--Thanks are due to several of my co- (edited by N. Hansen et al.), p. 15 (1981).
workers at Bochum who contributed micrographs from 22. K. Friedrich and E. Hombogen, J. Mater. Sci. IS.2175
their work for this paper and to Dr H. E. Exner, Stuttgart. (1980).
and Professor G. Ondraschek, Karlsruhe, for encouraging 23. R. Seifert and G. Wassermann. Z. Me~a~lk. 22.38 1,854
dirussions on microstructure. The work is supported by the (1981).
Federal Ministry of Research and Technology (BMFT- 24. Y. Huang, Concrere and Reinforced Concrete, China.
Project 03574/g). No. 5!6 ( f 982).