X-Ray Microbeam Measurement of Local Texture and Strain in Metals

Chung, J.-S.; Tamura, Nobumichi; Ice, Gene E.; Larson, B. C.; Budai, J. D.; Lowe, W. P.

doi:10.1557/proc-563-169

Cited by 18 publications

(8 citation statements)

References 10 publications

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“…It is described in detail in refs. [31,32,28,33]. The software automatically takes each pattern through image processing, peak indexing, strain refinement and stress determination steps using inputted crystal parameters and calibration to define the experimental geometry.…”

Section: X-ray Data Analysismentioning

confidence: 99%

Mapping mesoscale heterogeneity in the plastic deformation of a copper single crystal

Magid

Florando

Lassila

et al. 2009

Philosophical Magazine

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The work reported here is part of a 'multiscale characterization' study of heterogeneous deformation patterns in metals. A copper single crystal was oriented for single slip in the (111)[101] slip system and tested to ~10% strain in roughly uniaxial compression. The macroscopic strain field was monitored during the test by optical 'image correlation'. The strain field was measured on orthogonal surfaces, one of which (the x-face) was oriented perpendicular to [121] and contained the [101] direction of the preferred slip system. The macroscopic strain developed in an inhomogeneous pattern of broad, crossed shear bands in the x-face. One, the primary band, lay parallel to (111). The second, the 'conjugate' band, was oriented perpendicular to (111) with an overall (101) habit that contains no common slip plane of the fcc crystal. The mesoscopic deformation pattern was explored with selected area diffraction, using a focused synchrotron radiation polychromatic beam with a resolution of 1-3 µm. Areas within the primary, conjugate and mixed (primary + conjugate) strain regions of the x-face were identified and mapped for their orientation, excess defect density and shear stress. The mesoscopic defect structure was concentrated in broad, somewhat irregular primary bands that lay nominally parallel to (111) in an almost periodic distribution with a period of about 30 µm. These primary bands were dominant even in the region of conjugate strain. There were also broad conjugate defect bands, almost precisely perpendicular to the primary bands, that tended to bridge primary bands and terminate at them. The residual shear stresses were large (ranging to well above 500 MPa) and strongly correlated with the primary shear bands; interband stresses were small. The maximum resolved shear stresses within the primary bands were oriented out of the plane of the bands, and, hence, could not recover the dislocation structure in the bands. The maximum resolved shear stresses in the interband regions lay predominantly in {111} planes. The results are compared to the mesoscopic defect patterns found in Cu in etch pit studies done some decades ago, which also revealed a mesoscopic dislocation structure made up of orthogonal bands.

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Section: X-ray Data Analysismentioning

confidence: 99%

Mapping mesoscale heterogeneity in the plastic deformation of a copper single crystal

Magid

Florando

Lassila

et al. 2009

Philosophical Magazine

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“…The equipment described above enables us to keep the sample fixed and rotate the CCD to the desired position around the sample. A similar technique is used at the APS [7][8][9] and we apply it to both Al interconnects (this paper) and damascene Cu interconnects [10].…”

Section: Methodsmentioning

confidence: 99%

Grain Orientation and Strain Measurements in Sub-Micron wide Passivated Individual Aluminum Test Structures

Tamura

Valek

Spolenak³

et al. 2000

MRS Proc.

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An X-ray microdiffraction dedicated beamline, combining white and monochromatic beam capabilities, has been built at the Advanced Light Source. The purpose of this beamline is to address the myriad of problems in Materials Science and Physics that require submicron x-ray beams for structural characterization. Many such problems are found in the general area of thin films and nano-materials. For instance, the ability to characterize the orientation and strain state in individual grains of thin films allows us to measure structural changes at a very local level. These microstructural changes are influenced heavily by such parameters as deposition conditions and subsequent treatment. The accurate measurement of strain gradients at the micron and sub-micron level finds many applications ranging from the strain state under nano-indenters to gradients at crack tips. Undoubtedly many other applications will unfold in the future as we gain experience with the capabilities and limitations of this instrument. We have applied this technique to measure grain orientation and residual stress in single grains of pure Al interconnect lines and preliminary results on post-electromigration test experiments are presented. It is shown that measurements with this instrument can be used to resolve the complete stress tensor (6 components) in a submicron volume inside a single grain of Al under a passivation layer with an overall precision of about 20 MPa. The microstructure of passivated lines appears to be complex, with grains divided into identifiable subgrains and noticeable local variations of both tensile/compressive and shear stresses within single grains.

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“…Today, the availability of high brilliance third generation synchrotron sources, combined with progress in X-ray focusing optics and fast 2D large area detector technology have made possible the development of Scanning X-ray Microdiffraction (µSXRD) techniques using either monochromatic or polychromatic focused beams of sizes ranging from a few microns to submicron [1][2][3][4][5][6][7][8]. The closest equivalents in the electron microscopy field are STEM (Scanning Transmission Electron Microscopy) and EBSD (Electron Back Scatter Diffraction).…”

Section: Introductionmentioning

confidence: 99%

Submicron x-ray diffraction and its applications to problems in materials and environmental science

Tamura

Celestre

MacDowell

et al. 2002

Review of Scientific Instruments

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The availability of high brilliance 3 rd generation synchrotron sources together with progress in achromatic focusing optics allow to add submicron spatial resolution to the conventional century-old X-ray diffraction technique. The new capabilities include the possibility to map in-situ, grain orientations, crystalline phase distribution and full strain/stress tensors at a very local level, by combining white and monochromatic X-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron X-ray diffraction techniques at the ALS, we will give some examples of its application in material science for the measurement of strain/stress in metallic Work supported in part by the Department of Energy contract DE-AC03-76SF00515. August 2002 2 thin films and interconnects. Its use in the field of environmental science will also be discussed. KeywordsX-ray micro-diffraction, thin films, microtexture, strain/stress Contact Author Nobumichi Tamura, Lawrence Berkeley National Lab., MS 2-400, Berkeley, CA 94720, tel. (510) 486 6189, fax (510) 486 7696 e-mail: ntamura@lbl.gov Introduc tionMaterials properties such as strengthening, resistance to fatigue and failure intimately depend on their microstructural features such as grains, grain boundaries, inclusions, voids and other defects. However, at the so-called mesoscopic length scale (approximately between 0.1 and 10 microns) materials typically exhibit high inhomogeneity, and properties are extremely difficult to study both experimentally and theoretically. This length scale is situated between the atomic scale of atoms and individual dislocations, and the macroscopic scale of continuum mechanics.X-ray diffraction is a powerful technique, used for almost a century to measure grain orientation and strain, as well as for crystalline phase identification and structure refinement.Compared to electron microscopy, X-rays have the advantages of higher penetration depth (rendering possible the scanning of bulk and buried samples), do not require any particular sample preparation and can be used under a variety of different conditions (in air, liquid, 3 vacuum or gas, at different temperature and pressures). Its main drawback for the study of materials at the micron scale was until recently its poor spatial resolution.Today, the availability of high brilliance third generation synchrotron sources, combined with progress in X-ray focusing optics and fast 2D large area detector technology have made possible the development of Scanning X-ray Microdiffraction (µSXRD) techniques using either monochromatic or polychromatic focused beams of sizes ranging from a few microns to submicron [1][2][3][4][5][6][7][8]. The closest equivalents in the electron microscopy field are STEM (Scanning Transmission Electron Microscopy) and EBSD (Electron Back Scatter Diffraction).The spatial resolution of electron micr...

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X-Ray Microbeam Measurement of Local Texture and Strain in Metals

Cited by 18 publications

References 10 publications

Mapping mesoscale heterogeneity in the plastic deformation of a copper single crystal

Mapping mesoscale heterogeneity in the plastic deformation of a copper single crystal

Grain Orientation and Strain Measurements in Sub-Micron wide Passivated Individual Aluminum Test Structures

Submicron x-ray diffraction and its applications to problems in materials and environmental science

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