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SELFCONSISTENT DETERMINATION OF THE X-RAY ELASTIC CONSTANTS OF POLYCRYSTALLINE MATERIALS FOR ARBITRARY CRYSTAL SYMMETRY N. KOCH and H. WERN Laboratory of Computer Aided Applications, HTW des Saarlandes, University of Applied Sciences, Goebenstrasse 40, D-66117 Saarbrcken, Germany ABSTRACT For the calculation of load or residual stresses from measured strain data by means of x-rays or neutrons, the so called x-ray elastic constants are required. Usually they are calculated from the corresponding single crystal data assuming some models such as Voigt, Reuss or Krner. In this paper, the finite element method is used to guarantee both, stress equilibrium and strain compatibility across the grain boundaries. The method is applicable to materials with a random texture as well as to specimens with a given texture using the information of the Orientation Distribution Function (ODF). All crystal structures are supported. The method is demonstrated on trigonal Al2O3 and on textured thin films of Tungsten and Niobium. THEORY In x-ray stress analysis, one distinguishes between three different coordinate systems as illustrated in Figure 1. The material properties are usually defined in the crystallophysical coordinate system as shown in Figure 2. The angles and c are defined by the Miller indices under investigation of the corresponding single crystal structure. The angle is a free parameter, which defines an orientation about the hkl normal.

Specimen System S

SL

Laboratory System L

Crystallophysical System O

Figure 1: Coordinate systems used in x-ray stress analysis.

The xec`s are defined in the laboratory system. Therefore, the single crystal data have to be

O3
c

L3 || [hkl] O2

O1
Figure 2: Definition of the crystallophysical coordinate system associated to the single crystals.

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transformed into the laboratory system taking into account the transformation properties of a forth-rank tensor. The corresponding transformation matrix can be found in [1]. According to Nye2 the matrix notation of the elastic stiffness of trigonal single crystal coefficients reads as: C11 C12 C13 C14 C12 C11 C13 - C14 C13 C13 C33 C23 C14 - C14 C23 C14 C14 (C11 - C12)/2

(1)

where all entries marked with a dot are assumed to be zero. The angle describes the rotation of reflecting crystallites about the lattice plane normal (hkl). In a random material it is assumed, that the angle is equilibrated between 0 and 360 degrees. The theory for the determination of the so called quasiisotropic x-ray elastic constants s1(hkl) and s2/2(hkl) can be found in previous papers3-5. In the case of textured materials, the stress factors Fij have to be calculated. They are defined as (hkl ) Fij ( , , hkl ) = (2) _ ij They connect the strain determinable by diffraction methods to the mean phase stress within a textured material. For their calculation, the strains in the measuring direction have to be averaged considering all those crystals that contribute to the interference line. MODEL In order to fulfil the requirements of both stress equilibrium and strain compatibility across the grain boundaries, the finite element method is used to calculate the xecs. For that reason, a model is constructed which consists of 1000 three-dimensional hexahedrons representing the grains. Different grid sizes have been tested and the above coarsest number was chosen because the reproducibility of the results was in the order of 1%. The polycrystalline material is assumed to behave as a three-dimensional mixture of macroscopically isotropic and fully orthotropic grains where the relative ratio of both types can be chosen(in the present calculations always a factor of 50% was used). The macroscopic values of the compression and shear moduli K and G are calculated for any crystal structure according to an iteration procedure which was first proposed by Kneer6. The corresponding isotropic bulk moduli can 3K + 4G 3K - 2G B B then be calculated according to C11 = , C12 = . The orientations of the 3 3 orthotropic grains were defined in accordance with the requirements of the diffraction simulation described below. All grains were placed randomly in a mesh consisting of 8-noded hexahedrons. The far field load of 100 MPa was applied constant over the mesh boundary plane normal to a sample coordinate axis. In the case of the orthotropic grains, the orientation angles were assumed to be distributed in an equidistant manner between 0 and 360 degrees or are taken from the information of the ODF. The elastic moduli were rotated about the values to be coincident with the axes of the sample coordinate system. They were calculated for a given hkl reflection that would diffract at different tilts. In order to simulate a texture free random material, the number of reflecting crystallites for each -tilt was assumed to be equal whereas in textured materials, the number is dictated by the ODF.

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RESULTS In the present study, these calculations were carried out for the 006, 105, 104, 206, 114, 204, 123, 302, 121 and 100 reflections of trigonal Al2O3 in order to cover the full range of the orientation parameter. Because an ODF for this material was not available, it is handled as a random specimen. The corresponding single crystal as well as bulk data are summarized in table 1. Table 1: Elastic stiffness, shear and compression modulus in units of 1011 Pa7. 0 0 0 0 0 Crystal C11 G K C12 C14 C0 C13 C 33 44 Al2O3 4.95
10

c/a 2.7304

1.60

1.15

-0.23

4.97

1.46

1.625

2.517

Al2O 3
9 8

- s1 [ 10 MPa ]

-1

7 6 5 4 3 0,0 0,2 0,4 0,6 0,8 1,0

-7

Voigt Reuss Krner FE

Figure 3a: -s1 of Al2O3 versus orientation.

The results of the FE calculation are shown in Figure 3 together with the values according to the Voigt, Reuss and Krner model. The proof of Hill8 that the average elastic constants for a macroscopically isotropic aggregate should fall within the limits imposed by the Reuss and Voigt models is in accordance with the numerical results of the FE calculation. However, it should be recognized that the effectice xec`s need not to be within the Voigt and Reuss bounds, as was demonstrated by Leeuwen et al.9 by the sin2 plots for untextured and by Leoni et al.10 for textured films. For a textured specimen, the average strain in the measurement direction of the diffraction experiment is given by
2

()f ( )d
ij 0 2

f ()d
0

(3)

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4,5

Al2 O3
4,0

s2/2 [ 10 MPa ]

-1

3,5

-6

3,0

2,5

Voigt Reuss Krner FE

2,0 0,0 0,2 0,4 0,6 0,8 1,0

Figure 3b: s2/2 of Al2O3 versus orientation.

where f (hkl, , , ) is the representation of the ODF in terms of the measurement parameters. Three of such functions have been kindly provided by the MPI Stuttgart11. They have been calculated for a cubic crystal symmetry assuming a Gaussian <110> fibre texture with 50 HWHM and are shown in Figure 4.
40

(a) = 52

(b) = 88
30

f( )

f( )
10 0 0 40 80 120 160 200 240 280 320 360 0

20

40

80

120

160

200

240

280

320

360

[degrees]

[degrees]

16

(c) = 74

12

Figure 4: Relative intensity of the ODF(Gaussian <110> fibre texture; 50 HWHM) as functions of the rotation around the diffraction vector (a), (b) for the (110) reflection at (a) =520, (b) =880 and (c) for the 321 reflection at =740.

f( )

40

80

120

160

200

240

280

320

360

[degrees]

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In order to check the feasibility of the method. the stress factor F11 has been calculated for all reflections of the Tungsten mesh, because Tungsten is the prototype of an elastically isotropic material with an anisotropy index equal to 1. The result shows a perfect linear variation of all grains and is the same for all reflections both for a random or preferred orientation. This indicates that the formalism is working as expected. Table 2: Single crystal elastic constants in units of 1011 Pa12 and anisotropy factor A. 0 0 Crystal A C11 C12 C0 44 W Nb 5.01 2.446 1.98 1.381 1.514 0.292 1.0 0.55

2,5 2,0 1,5

W Random ODF

F11 [10 MPa ]

-1

1,0 0,5 0,0 -0,5 -1,0 0,0 0,2 0,4 0,6 0,8 1,0

-6

sin ( )

Figure 5: Calculated stress factor F11(=00) of the {110} reflection of Tungsten .

The corresponding result for the Nb mesh is shown in Figure 6 for the {110} reflection.
10 8 6

Nb Random ODF

F1 1[10 -6 MPA-1]

4 2 0 -2 -4 -6 0,0 0,2 0,4 0,6 0,8 1,0

sin ( )

Figure 6: Calculated stress factor F11(=00) of the {110} reflection of Niobium.

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Because of the elastic anisotropy there is a deviation from linearity. The squared symbols correspond to the analysis of a random distribution. A linear least squares analysis shown as a straight line would result in the quasiisotropic elastic constants s1 and s2/2. By use of the ODF (Fig. 4a,b), the corresponding FE results for =520 and =880 are also shown as a circle. The deviation of the stress factor from a random distribution is in the order of about 10%. For the {321} reflection the effect is less pronounced as can be seen by inspection of Figure 7 where the local stress is shown as a function of sin2.
120 115

Local stress along S1 [MPa]

110 105 100 95 90 85 80 0,0 0,2

Nb 321 reflection Random ODF

s a pp = 100 MPa

0,4

0,6
2

0,8

1,0

sin ()

Figure 7: Variation of the local stress along S1 in the grains diffracting at various angles.

CONCLUSION A selfconsistent approach using the method of finite elements allows an ab initio calculation of the x-ray elastic constants from the single crystal elastic constants. In the case of a random distribution of the reflecting crystallites within macroscopically isotropic bulk material, the {hkl}dependent and so called quasiisotropic x-ray elastic constants are obtained. In textured materials, the explicit information of the ODF is used to calculate the corresponding stress factors. REFERENCES [1] C.M. Brakman, J. Appl. Cryst. 16, 325 (1983). [2] J.F. Nye, Physical Properties of Crystals, Oxford University Press, 1985. [3] D. Chidambarrao, Y.C. Song and I.C. Noyan, Metall. Mater. Trans. A, 28A, 2515 (1997). [4] H.Wern and C. Funk, Materials Science Forum Vols. 347-349, 199 (2000). [5] H.Wern, T. Maas and N. Koch, Adv. In X-Ray Anal. 44 (2000). [6] G. Kneer, Dissertation, Bergakademie Clausthal (1964). [7] T. Sasaki, Kanazawa University, private communication. [8] R. Hill, Proc. Phys. Soc. A65, 349 (1952). [9] M. van Leeuwen, J.-D. Kamminga and E.J. Mittemeijer, J. Appl. Phys., 86, 1904 (1999). [10] M. Leoni, U. Welzel, P. Lamparter, E.J. Mittemeijer and J.D. Kamminga, Phil. Mag. A , 81, 597 (2001). [11] U. Welzel, Max Planck Institute for Metals Research, Stuttgart, private communication. [12] M.A. Meyers and K.K Chawla, Mechanical Metallurgy, Principles and Applications, Prentice-Hall, 1984.