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1827±1836, 1998
Acta Metallurgica Inc.
Published by Elsevier Science Ltd
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AbstractÐThe relation between polycrystal deformation and single crystal deformation has been studied in
this work. A pure aluminium polycrystal having an average grain size of 300 mm has been strained in ten-
sion at room temperature. The ¯ow stress has been determined at four dierent strains (0.05, 0.14, 0.22
and 0.34) and deformation microstructures have been characterized qualitatively and quantitatively by
transmission electron microscopy. Improved experimental techniques have allowed large foil areas to be
characterized and in total 89 grains have been examined. At the four strains examined a classi®cation of
the deformation microstructures into three dierent types has shown a correlation between the grain orien-
tation and the type of deformation microstructure which develops during straining. The dislocation density
has been calculated at each strain and by assuming that the shear stress is proportional to the square root
of the dislocation density the shear stress±strain relationship has been derived for each of the three groups
of grains showing dierent deformation microstructures. The stress±strain curves show a strain hardening
behaviour which depends on the orientation of the grain. The behaviour of the grains embedded in the
polycrystal is compared with the behaviour of single crystals and the stress±strain curve of the polycrystal
is estimated with good accuracy from single crystal data, which are weighted based on a quantitative tex-
ture analysis of the polycrystal. # 1998 Acta Metallurgica Inc.
15, 25 and 40%). The strain rate used was where Sv is the dislocation boundary area per unit
8.3 10ÿ4 sÿ1. To ensure that the stress±strain beha- volume and rA is the dislocation density per unit
viour is representative for true polycrystalline beha- area of boundary [14]. Sv does not depend on the
viour the stress±strain curve has been compared spatial arrangement of the boundaries and equals
with previous data obtained from specimens having 2/Dr [13]. rA equals 1/h for a simple tilt wall where
a larger ratio between the specimen cross section h is the spacing between the dislocations and for a
and the grain size [10]. Very good agreement has twist wall rA=2/h [15]. For small angles of misor-
been found both in shape and level of the stress±
ientation h 2 b/ym and by averaging over tilt and
strain curves indicating that an eect of surface
twist boundaries rA is approximated by 1.5 ym/b.
grains is negligible in the present specimens. For
transmission electron microscopy (TEM) obser- The dislocation density in the boundaries is then:
vations, thin foils have been cut from the two side rb 3ym =Dr b
2
planes of the tensile specimens and subsequently
thinned and electropolished using standard Besides the dislocations present in dislocation
methods. In this preparation, care has been exerted boundaries, dislocations are also found in the
in obtaining foils from the interior of the specimens volumes between the boundaries. The density of
to reduce possible surface eects. On each foil the these dislocations (ro) has been determined from
tensile axis has been marked allowing the orien- TEM micrographs by counting the number of inter-
tation of crystallites to be determined with respect sections between dislocations and a set of random
to this axis. In order to obtain accurate structural test lines (PL). The dislocation density is then
parameters large areas have been examined of the
order of 2000±6000 mm2 of each grain. In total 89 ro 2PL =t
3
grains have been examined at the four strains. where t is the foil thickness [13]. This parameter has
Local orientation measurements of crystallites
been determined from intensity oscillations in con-
within grains have been made using a semiauto-
vergent beam diraction patterns. In general, the
matic Kikuchi line technique in the areas where the
determination of ro is not very accurate but as ro is
montages of the microstructure are taken [11].
Linear and area scanning have been used when only a rather small fraction of the total dislocation
measuring the orientation of the crystallites allow- density, the accuracy of measuring the dislocation
ing the orientation measurement to be related to density is predominantly determined by the pre-
the microstructural observations. One such relation- cision in measuring ym and Dr.
ship concerns the crystallographic characteristic of The texture of the tensile specimens in the unde-
the boundaries in which the dislocations have accu- formed state and after straining has been deter-
mulated, i.e. a dislocation boundary should be mined by neutron diraction [16]. For each sample
classi®ed as either a crystallographic or a non-crys- three complete pole ®gures have been measured and
tallographic boundary [12]. A boundary in the ®rst the three-dimensional crystallite orientation distri-
category is taken to be parallel to within 58 with a bution function (ODF) has been calculated using
slip plane, whereas boundaries in the second cat- the series expansion method [17]. Table 1 shows the
egory make a larger angle with a slip plane. A pre-
volume fractions for the [100], [111] and [110] orien-
liminary classi®cation is based on measurements of
tations which have been determined by integrating
the angle between the dislocation boundary and the
the density over an angle of 158 around the ideal
trace of the slip plane in the ®eld of observations.
The analysis was then re®ned by tilting the foil to position of the component in the stereographic tri-
achieve the minimum image width for the dislo- angle. Table 1 shows that the texture changes are
cation boundaries. The inclination of this boundary not very pronounced over the strain range investi-
plane to the nearest slip plane was then determined gated. There is a tendency that the [111] component
and if the inclination was determined to be less strengthens and that the [110] component weakens.
than 58 than the boundary was con®rmed as of This corresponds well to predictions by the Taylor
crystallographic type. model [2, 5] that unstable crystal orientations rotate
The orientation measurements are used to calcu- towards either [100] or [111] directions for straining
late the mean misorientation angle (ym) across the in tension.
dislocation boundaries. Also the spacing between
the boundaries (Dr) is determined by counting the Table 1. Volume fractions of texture components
number of intersections between the boundaries and
h100i h111i h110i
a random set of test lines [13]. From the two Strain 0±158 0±158 0±158
parameters ym and Dr the volume density of dislo-
0 0.280 0.132 0.100
cations in boundaries (rb) can be obtained from the 0.05 0.240 0.109 0.106
equation: 0.14 0.282 0.236 0.048
0.22 0.256 0.284 0.023
rb Sv rA
1 0.34 0.277 0.226 0.033
HANSEN and HUANG et al.: MICROSTRUCTURE AND FLOW STRESS 1829
Fig. 5. Inverse pole ®gure as in Fig. 4, but subdivided into ®ve regions (see text).
HANSEN and HUANG et al.: MICROSTRUCTURE AND FLOW STRESS 1831
Table 2. Volume fractions ( f ) and average M-factors for three groups of grains showing dierent types of deformation microstructure
Type 1 Type 2 Type 3
Strain f1 M1 f2 M2 f3 M3
grains have been calculated, see Table 2. In this cal- above 0.2 in the dislocation density of grains with
culation it has been assumed that the texture of the Type 2 structures, i.e. grains with orientations near
specimens shows rotational symmetry. This intro- the h100i corner position in Fig. 4. From the dislo-
duces a discrepancy when comparing with calcu- cation density and the volume fraction (Table 2) of
lations where the full ODF information is used. A the three groups of grains, the total dislocation den-
comparison shows that this discrepancy is small sity (rt) of the specimen can be calculated. rt is
about 3%, and it has therefore been neglected. given in Table 3 together with the measured tensile
Table 2 shows that neither the volume fraction nor ¯ow stress.
the M-values are much aected by the tensile strain. The ¯ow stress in terms of the resolved shear
However, this does not mean that grain rotations stress (t) has been estimated for the three types of
have not taken place during straining. This is illus- structures based on the empirical relation by taking
trated in Fig. 6 showing the volume concentrations the friction stress to, equal to zero and applying
of grains in the ®ve regions in Fig. 5. Figure 6 p
clearly shows that the concentration of grains near t abG ro rb
4
the boundary line between [100] and [111] increases
where b is Burgers vector (b = 0.286 10ÿ9 m), G is
with strain in accordance with model predictions
the shear modulus (G = 26,000 MPa), and a is a
(see Section 2). Also to be noted in Fig. 6 is that
the largest changes appear to be rotations from number of the order of 0.2±0.35 [19, 20]. The val-
region 5 to region 4, i.e. the grains rotate through idity of equation (4) has been shown in many stu-
orientations, all representing the group of grains dies and apart from a variation in a, equation (4) is
developing the Type 3 microstructure. quite insensitive to changes in materials and process
parameters. In order to derive an estimate of a in
the present experiment, equation (4) has been used
3.3. Dislocation density and ¯ow stress to calculate the ¯ow stress (s) of the polycrystalline
For each of the three groups of grains the dislo- specimen taking s = Mt, thus
cation density (rb+ro) has been determined as a p
s MabG rt
5
function of strain, see Fig. 7. It is estimated that
the densities given are determined with an accuracy where M is the average Taylor factor which is cal-
of about 10% and it should be noted that rb only culated to 2.94 from M-factors for three groups of
accounts for the geometrically necessary dislo- grains and for four strains (Table 2). The data in
cations. Figure 7 shows that the dislocation density Table 3 allows a calculation of a, which also is
of grains with Type 3 structures is signi®cantly lar-
ger than that of grains with Type 1 and Type 2
structures. Also note the small increase for strains
Table 3. Flow stress and dislocation density nominal shear stress±strain behaviour for the poly-
Dislocation crystal, using an M factor of 2.94 when transform-
Tensile Tensile ¯ow density ing from tensile stress/strain to shear stress/strain.
strain stress (MPa) 1013(mÿ2) a
Here, the strain hardening behaviour of the poly-
0.05 34.9 3.2 0.28 crystal diers signi®cantly from the behaviour of
0.14 48.5 9.8 0.22 the three groups of grains which together comprises
0.22 55.2 15.1 0.21
0.34 61.5 19.0 0.20 the structure of the polycrystalline specimen.
G = 26,000 MPa; b = 0.286 10ÿ9 m; M = 2.94.
4. DISCUSSION
given in Table 3. a is observed to decrease with
strain, but a reasonable approximation of the exper- This experiment shows for grains embedded in a
imental stress±strain curve can be obtained for the polycrystal a clear correlation between the crystallo-
average value of a equal to 0.24, which will be used graphic orientation, the deformation microstructure
and the estimated shear stress±strain behaviour.
in the following. The good agreement between this
This has also been observed for single crystals
®gure and the a-values reported in the literature
deformed in tension where the microstructure [21±
(e.g. Refs [18] and [19]) gives good con®dence in the
27] and the shear stress±strain behaviour [3, 4, 28±
applied method of determining the dislocation den-
31] has been examined for dierent crystal orien-
sity. That the experimental a value of 0.24 is rela-
tations. A comparison between polycrystalline beha-
tively low compared to published values indicates viour and single crystal behaviour will therefore be
that the contribution to the total dislocation density carried out in the following based on (i) microstruc-
from geometrically necessary dislocations appar- tural observations and (ii) estimates and measure-
ently outweighs the contribution from redundant ments of the stress±strain behaviour. This
dislocations in the boundaries. comparison is followed by a discussion of polycrys-
The shear stress for the grains having the three tal deformation, especially the stress±strain curve of
dierent types of microstructure is plotted in Fig. 8 the polycrystal.
vs the shear strain. This strain has been estimated
by multiplying the tensile strain with an average 4.1. Microstructure and slip pattern
M factor for each of the three groups of grains Deformation microstructures have not been stu-
averaged over four strain values. These died to a great extent in aluminium single crystals
factors are M1(av) = 2.76, M2(av) = 2.40 and strained in tension. Copper crystals are, however,
M3(av) = 3.26 (Table 2). Note in Fig. 8 that three expected to show a comparable behaviour and such
groups of grains having the three dierent types of crystals have been studied in more detail [21±26]. A
microstructure show signi®cantly dierent shear general ®nding has been [21±24] that the defor-
stress±strain curves. Most marked is the typical mation structure of the [100] crystal is a character-
Stage ``III'' behaviour, i.e. parabolic hardening of istic three-dimensional, uniform cell structure,
group 3 grains compared to the behaviour of group whereas a banded structure of dislocation bound-
2 grains where a rapid strain hardening at low aries is generally observed for other
strain develops into a low hardening region at med- orientations [24±26]. For such banded structures it
ium to high strain. In Fig. 8 is also plotted the has been found that the deviations of the plane of
the dislocation boundary from the primary slip
plane increases with increasing multiplicity of slip.
An example of this eect is a deviation of 298
measured for the dislocation boundaries in a [111]
crystal, which has six slip systems [25]. These obser-
vations have been further examined by a Schmid
factor analysis [27], which shows that if two systems
on one or two planes have high Schmid factors the
crystals tend to form crystallographic dislocation
boundaries. However, if more than two slip planes
have high Schmid factors, the crystals tend to form
non-crystallographic boundaries [27].
For the present polycrystal, a Taylor analysis in
general agrees with a Schmid factor analysis for
single crystals as the group of grains developing
Type 1 structures predominantly slip on two planes,
whereas the group of grains developing Type 3
Fig. 8. The shear stress±strain curves for groups of grains
structures slip on three or more planes. For the
having dierent types of microstructure (see text) and for group of grains developing the Type 2 structure the
the polycrystalline specimen. number of slip planes is four as in a [100] single
HANSEN and HUANG et al.: MICROSTRUCTURE AND FLOW STRESS 1833
Fig. 10. The nominal shear stress±strain curve for grains Fig. 12. The nominal shear stress±strain curve for grains
having Type 1 microstructure compared with the stress± having Type 3 microstructure compared with the stress±
strain curve for two crystals numbers 14 and 15 in Ref. strain curves for a [111] crystals from Ref. [31].
[30] having an orientation on the boundary between [100]
and [111] in the standard triangle [30].
Fig. 13. Tensile ¯ow stress±strain curves for single crystals of corner orientations ([100] and [111]) from
Ref. 31 and of an orientation crystals numbered 14 and 15 in Ref. [30] on the boundary between [100]
and [111]. (The latter curve has been obtained by transforming the shear stress±strain curve in Fig. 10
by the use of a Taylor-factor equal to 2.8.) The contributions of the three single crystals to the tensile
¯ow stress of a polycrystalline specimen have been weighted and added to give the curve marked
Polycryst. (calc.). On this ®gure is also shown the tensile stress±strain curve for the polycrystal tested in
this work, marked Polycryst. (exp.).
activation of extra slip systems near grain bound- M-factor for an ideal h111i crystal which is 3.67
aries and triple junctions. (18) and the average M-factor for group 3 grains
Based on the observed correlations between poly- which is 3.26. The calculated curve is shown in
crystalline and single crystal behaviour the polycrys- Fig. 13 together with the experimental stress±strain
talline tensile stress±strain curve may be calculated curve for the polycrystalline specimens. Good agree-
based on the stress±strain curves for single crystals, ment is observed both when it comes to the shape
see Fig. 13. This calculation of the stress±strain of the curve and the magnitude of the ¯ow stress,
curve of the polycrystal is based on the assumption although there is a certain overprediction of the
that the contribution for the three groups of grains ¯ow stress at large strain.
of the polycrystal can be added linearly after being
In the calculation of the polycrystalline curve in
weighted based on the volume fractions given in
Fig. 13 a contribution of grain boundary strength-
Table 2. It is further assumed as in the Taylor
ening is not included. This contribution is, however,
model that the tensile strain is the same for the
not large, of the order of 3±4 MPa for the present
embedded grains of the polycrystal as for the bulk
grain size [10].
polycrystalline specimen.
The polycrystalline curve is calculated by using In conclusion, it appears to be a crucial obser-
the crystals numbered 14 and 15 in Ref. [30] and vation that the stress±strain behaviour of grains in
the [100] curve to calculate the contributions of a polycrystal is orientation dependent and shows
grains of group 1 and group 2, respectively. No cor- many similarities with single crystals oriented for
rection is made for the change in the Taylor M-fac- double slip and multislip. To explore the relation-
tor as it is quite similar for the single crystals 2.8 ship between polycrystals and single crystals, the
and 2.45, respectively and for the groups of behaviour of grains embedded in a polycrystal must
embedded grains of the polycrystal 2.76 and 2.40, be studied further and also as a function of the
respectively (from Table 4). For grains of group 3 grain size. Such investigations can be greatly facili-
the h111i curve is used, however, after an M-factor tated, if the grains in the polycrystal can be classi-
correction due to the signi®cant dierence in the ®ed into groups showing a similar microstructural
and mechanical behaviour. A microstructural analy-
Table 4. M-factors sis can be used in these studies, but a faster tech-
Type of grain M-factor nique is desirable. One such technique is high-
14, 15 crystals* 2.8 (estim.)
energy X-ray diraction, where the behaviour of in-
[100] crystal 2.45 dividual grains embedded in a polycrystal can be
[111] crystal 3.67 studied both during and after deformation [34]. Of
Group 1 grains 2.76 (aver.)
Group 2 grains 2.40 (aver.) special interest will be the combined observations of
Group 3 grains 3.26 (aver.) microstructural and crystallographic changes during
*See text and Ref. [30]. in situ deformation of embedded grains in poly-
1836 HANSEN and HUANG et al.: MICROSTRUCTURE AND FLOW STRESS
crystals which may then be compared with the 7. Aernoudt, E., Gil, Sevillano J. and Van Houtte, P., in
behaviour of single crystals. Constitutive Relations and Their Physical Basis, ed. S.
I. Andersen, J. B. Bilde-Sùrensen, N. Hansen, T.
Leers, H. Lilholt, O. B. Pedersen and B. Ralph. Risù
5. CONCLUSIONS National Laboratory, Roskilde, 1987, p. 1.
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Pure aluminium polycrystals have been strained in Numerical Predictions of Deformation Processes and
in tension at room temperature and based on a the Behaviour of Real Materials, ed. S. I. Andersen, J.
B. Bilde-Sùrensen, T. Lorentzen, O. B. Pedersen and
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have been reached: 1994, p. 33.
9. Hansen, N., Metall. Trans., 1985, 16A, 2167.
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stress proportional to the square root of the dis- Pedersen and N. J. Sùrensen. Risù National
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AcknowledgementsÐWe thank Drs B. Bay, J. B. Bilde- 23. Ambrosi, P., GoÈttler, E. and Schwink, Ch, Scripta
Sùrensen, D. A. Hughes, D. Juul Jensen, Q. Liu, Y. L. Metall., 1974, 8, 1093.
Liu, and T. Leers for many fruitful discussions. J. 24. Kawasaki, Y., Jap. J. Appl. Phys., 1979, 18, 1429.
Lindbo is gratefully acknowledged for his very skilled 25. Kawasaki, Y. and Takeuchi, T., Scripta Metall., 1980,
preparation of the TEM foils. Finally, we thank T. Skov 14, 183.
for drawing the ®gures and E. Sùrensen for typing the 26. Kawasaki, Y., in Strength of Materials, ed. H.
manuscript. The present work is performed under the Oikawa, K. Maruyama, S. Takeuchi and M.
Danish Materials Technology Programme ®nanced by the Yamaguchi. The Jap. Inst. of Metals, 1994, p. 187.
Danish Agency for Development of Trade and Industry, 27. Liu, Q. and Hansen, N., Phys. Stat. Sol. (b), 1995,
The Danish Natural Science Research Council and the 149, 187.
Danish Technical Research Council. 28. LuÈcke, K. and Lange, H., Z. Metallk., 1952, 43, 55.
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