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Applications of Texture Analysis

Ceramic Transactions, Volume 201

A Collection of Papers Presented at the 15th International Conference on Textures of

Materials (ICOTOM 15) June I-6,2008

Pittsburgh, Pennsylvania

Edited by A. D. Rollett

A John Wiley 81 Sons, Inc., Publication

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Ceramic Transactions, Volume 201

A Collection of Papers Presented at the 15th International Conference on Textures of

Materials (ICOTOM 15) June I-6,2008

Pittsburgh, Pennsylvania

Edited by A. D. Rollett

A John Wiley 81 Sons, Inc., Publication

Copyright 0 2009 by The American Ceramic Society. All rights reserved.

Published by John Wiley & Sons, Inc.. Hoboken, New Jersey. Published simultaneously in Canada.

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Contents

Preface

Acknowledgments

xv

xvii

THIN FILMS (MICROELECTRONICS, HTSC)

The Texture of Thin Nisi Films and Its Effect on Agglomeration 3 K. De Keyser, C. Detavernier , R. L. Van Meirhaeghe, J. Jordan-Sweet, and C. Lavoie

Epitaxial Substrates from Ni-Based Ternary Alloys With Cr and W 11 D.P. Rodionov, I.V. Gervasyeva, Yu.V. Khlebnikova, and V.A. Kazantsev

Cube Texture Formation in Ni-Pd and Ni-Pd-W Alloys For HTS Tapes

23

I.V. Gervasyeva, D.P. Rodionov, Yu.V. Khlebnikova, G.A. Dosovitskii, and A.R. Kaul

Texture of Rapidly Solidified Cu Thin Films Studied by SEM EBSD 35 and TEM

R. Zhong, A. Kulovits, J.M.K. Wiezorek, and J.P. Leonard

Control of Texture in Polycrystalline Thin Films Used as Data Storage Media

David E. Laughlin, Hua Yuan, En Yang, and Chun Wang

Influences of Processing Parameters on Microstructures and Microtextures of Au Flip Chip Bonds During Microelectronics Packaging

P Yang, C-M Li, D-M Liu, M Hung, M Li, and W-M Mao

47

57

V

TEXTURE AT NON-AMBIENT CONDITIONS

In Situ Observation of Texture Evolution in Ti-10-2-3 65 Seerna L. Raghunathan, Richard Dashwood, Martin Jackson, Sven Vogel, and David Dye

Study of Texture Evolution at High Strain Rates in FCC Materials 73 Nilesh Gurao, Satyam Suwas, and Rajeev Kapoor

Texture and Microstructure Development in Copper after Cryogenic Rolling and Heat Treatment

A. Haldar, D. Das, and P.P. Chattopadhyay

In-Situ EBSD Study of the a-y-a Phase Transformation in a Microalloyed Steel

Lischewski, D. M. Kirch, A. Ziemons, and G. Gottstein

Texture Changes during Phase Transformations Studied In Situ With Neutron Diffraction

Hans-Rudolf Wenk

NOVEL TEXTURE MEASUREMENT TECHNIQUES INCLUDING 3D

Three-Dimensional FIB-OIM of Ceramic Materials Shen J. Dillon and Gregory S. Rohrer

Comparison of X-Ray and EBSD Textures for Back-Annealed AI-Mg Alloys

0. Engler

83

95

103

117

125

A New Method for Quantification of Texture Uniformity of Plate 135 Peter Jepson and Robert Bailey

Separating Coincident Electron Backscatter Diffraction Patterns Near Interfaces

Josh Kacher, Brent L. Adarns, David Fullwood, and Colin Landon

147

Rapid Texture Determination Based on Two Dimensional X Ray Detector

Weimin Mao

155

Semiautomatic Determination of Orientations and Elastic Strain from Kossel Microdiffraction

163

Adam Morawiec, Raphael Pesci, and Jean-Sebastien Lecomte

vi . Applications of Texture Analysis

Statistically Reliable EBSD Analysis Method of Grain Boundary Characterization

D.H. Kim, J.Y.Kang, D.I. Kim, E.K. Her, S.J. Kim, H.N. Han, K.H. Oh, and H.C. Lee

3D Microstructures and Textures of a Plane Strain Compressed (1 10}4 12> AI-0.3% Mn Single Crystal

H. Paul, J.H. Driver, and CI. Maurice

Three Laws of Substructure Anisotropy of Textured Metal Materials, Revealed by X-Ray Method of Generalized Pole Figures

Yuriy Perlovich, Margarita Isaenkova, and Vladimir Fesenko

3D-Microstructural and Texture Characterization in Different Length Scales

Roumen Petrov and Patricia Gobernado Hernandez, Orlando Leon Garcia, Hemant Sharma, and Leo Kestens

Local Crystal Rotations of Bulk Grains by High-Resolution EBSD during Hot PSC of AI-0.1 % Mn Polycrystals

Romain Quey, David Piot, and Julian Driver

Grain Boundary Orientations in a Fe-Mn-Cu Polycrystalline Alloy M. Takashima and P. Wynblatt

Development of a TEM-Based Orientation Microscopy System S. Zaefferer and G. Wu

COMPLEX OXIDES AND OTHER COMPOUNDS

Domain Control Effect on Voltage-Strain in BaTi03 Single Crystal Yoshio Akimune, Kazuo Matsuo, Ryutaro Oishi, and Akira Okada

Tentative Simulation of Crystal Rotation for NaCl Structures Hiroaki Masui

INTERFACE TEXTURES

Grain Boundary Patterns in Dynamically Recrystallized Quartz Aggregates

Cristiane Castro and Leonard0 Lagoeiro

The Correlation between Grain Boundary Character and lntergranular Corrosion Susceptibility of 21 24 Aluminum Alloy

L. H. Chan, H. Weiland, S. Cheong, G.S. Rohrer, and AD. Rollett

171

181

189

197

205

21 3

221

231

239

251

261

Applications of Texture Analysis . vii

Rodrigues-Frank Spaces for Misorientations and Orientation Relationships between Crystals of Any Two Crystallographic Point Groups

269

Youliang He and John J. Jonas

Origins of Texture Memory in Steels Bevis Hutchinson and Leo A.I. Kestens

281

A Grain Boundary Analysis of Cemented Tungsten Carbides using OIM

Vineet Kumar, Zhigang Zak Fang, S.I. Wright and M.M. Nowell

291

The Effect of Grain and Phase Boundary Misorientation on Nucleation during Solid-state Phase Transformations in a Co-l5Fe Alloy

305

H. Landheer, S.E. Offerman, and L.A.I. Kestens, T. Takeuchi, M. Enomoto, and Y. Adachi

Microstructural Modification in a 150-1 5Ni-2.2 Mo-Ti Modified Austenitic Stainless Steel through Twin Induced Grain Boundary Engineering

31 3

Sumantra Mandal, P.V. Sivaprasad, and V. Subramanya Sarrna

Effect of Strain Path and Annealing on Development of Resistance to lntergranular Degradation in Austenitic Stainless Steels

323

V. Randle, R. Jones, T.J. Marrow, and D. Engelberg

Evolution of the Grain Boundary Character Distribution in 335 Strontium Titanate during Grain Growth

Herbert M. Miller and Gregory S. Rohrer

A Model for the Origin of Anisotropic Grain Boundary Character 343 Distributions in Polycrystalline Materials

Gregory S. Rohrer, Jason Gruber, and Anthony D. Rollett

Nucleation of the Primary A1 Phase on TiA13 during Solidification 355 of a Hot-Dip Zn-1 1 %A1-3%Mg-On2%Si Coating on Steel Sheet

Kazuhiko Honda, Kohsaku Ushioda, and Wataru Yamada

RECRYSTALLIZATION TEXTURE: RETROSPECTIVE VERSUS CURRENT PROBLEMS

Textural lnhomogeneity Effect during the Monte Carlo Simulation of the Abnormal Goss Grain Growth in Fe-3%Si Steel Grade HiB

365

T. Baudin, R. Penelle, and D. Ceccaldi

viii . Applications of Texture Analysis

Avoiding Roping and Ridging in AA6XXX Sheets: Characterizing the Initial State

T.A. Bennett, R.H. Petrov, and L.A.I. Kestens

Development of Cube Texture in Cold-Rolled and Annealed Multilayer Tapes for Coated Superconductor Applications

P.P. Bhattacharjee and R.K. Ray

Effects of Elastic Modulus on Deformation and Recrystallization of High Purity Nb

D. Baars, H. Jiang, T.R. Bieler, A. Zamiri, F. Pourboghrat, and C. Compton

Through-Process Texture Modeling of AA6016 from Hot Rolling to Final Annealing

C. Bollmann and G. Gottstein

Cube Texture Due to Dynamic Recrystallization in Pb and Pb-62%Sn Alloys under Equal Chanel Angular Extrusion Processing

R.E. Bolmaro, V.L. Sordi, M. Ferrante, WeiMin Gan, and H.-G. Brokmeier

Annealing Texture Evolution I.L. Dillamore

On the Stability of Recrystallization Textures in Low Alloyed Zirconium Sheets

FranCois Gerspach, Nathalie Bozzolo, and Francis Wagner

An Analysis of the Texture and Mean Orientation of Aluminium Alloy AA5052 Subjected to Forward and Reverse Hot Torsion and Subsequent Annealing

0. Hernandez-Silva, B.P. Wynne, and W. M. Rainforth

Evolution of { l l l } Recrystallization Texture in Al-Mg-Si Alloy Sheets Processed by Symmetric and Asymmetric Combination Rolling

Hirofumi Inoue, Satoshi Kobayashi, Masayuki Hori, Toshio Komatsubara, and Takayuki Takasugi

Effect of External Constraint and Deviation from Ideal Orientation on Development of Rolling Texture in Pure Aluminum Single Crystal Having {loo} Orientation

Keizo Kashihara and Hirosuke lnagaki

Nucleation and Growth of New Grains in Deformed Quartz Single Crystals

Leonard0 Lagoeiro and Paola Barbosa

373

381

391

399

409

42 1

429

437

445

453

46 1

Applications of Texture Analysis . ix

Rolling and Annealing Textures of Silver Sheets Dong Nyung Lee, Heung Nam Han, and Se-Jong Kim

Function of Layer Thickness on the Microstructural Evolution in Copper of Annealed Roll-Bonded CuNb Composites

S.C.V. Lim and A.D. Rollett

Influence of Taylor Factor M on Recrystallization of The Cube and Cube-Family Grains in FCC Metal

Hiroaki Masui

Multi-Cycle Pinch Welding of 304L Tubes: lnhomogeneities in Deformation and Recrystallization Textures and Microstructures

C.T. Necker, A.N. Marchi, and M.G. Smith

Effect of Mg Concentration on Texture Formation in AI-Mg Alloys during High Temperature Compression

Kazuto Okayasu, Hiroki Takekoshi, Masayuki Sakakibara, and Hiroshi Fukutomi

Ultra-Fine Grain Austenitic Stainless Steels: Influence of Texture during Recrystallization

Angeline Poulon-Quintin, Stephanie Brochet, Jean-Bernard Vogt, Jean-Christophe Glez, and Jean-Denis Mithieux

Patterns of Deformation and Associated Recrystallization in Warm/Hot Deformed AA6022

S. Raveendra, S. Mishra, H. Weiland, and I. Samajdar

Studies on Texture and Microstructure of Cryorolled and Annealed Cu-5%AI, Cu-5%Zn Alloys

V.L. Niranjani, Nilesh Gurao, U. Wendt, S. Suwas, and V. Subramanya Sarma

Modeling of Texture Development during Tandem Hot Rolling of AA3 1 03

C. Schafer, V. Mohles, and G. Gottstein

Texture Modification in Asymmetrically Rolled Aluminum Sheets Jurij Sidor, Roumen Petrov, Alexis Miroux, and Leo Kestens

In-Situ SEM/EBSP Analysis during Annealing in AI-Mg Alloys Yoshimasa Takayama, Kazuhiro Morita, Hajime Kato, and Yoshimasa Ookubo

Oriented Grain Growth and the Effect of In-Situ Annealing on Texture in AlMn Alloys

Caterina E. Tommaseo and H. Klein

469

481

489

499

507

51 5

523

529

537

547

555

561

x . Applications of Texture Analysis

Subgrain Coarsening of Hot-Rolled AA5005 Aluminum Alloy: A Comparison between EBSD Observations and Monte Carlo

Shengyu Wang, Mohammed H. Alvi, and Anthony D. Rollett

Influence of Low Angle Grain Boundaries on Recrystallization Myrjam Winning and Dierk Raabe

BIOMATERIALS

Comparison of Calcite Crystallographic Texture in the Shells of the Rhynchonelliform Brachiopod, Terebratulina Retusa and the Bivalve Mollusc, Mytilus Edulis

M.Cusack, A. Perez-Huerta, P. Dalbeck, P. Chung, and M.R. Lee

Wear Resistance and Texture Evolution of Ultra High Molecular Weight Polyethylenes during Uniaxial Compression

D.S. Li, H. Garmestani, S.C. Davis, L.K. Moss, A.K. Siddiqi, J.B. Guthrie, N. Johansen, and L. Matrisciano

Texture and Microstructure of Modern Rhynchonellide Brachiopod Shells-An Ontogenetic Study

E. Griesshaber, R.D. Neuser, U. Brand, and W.W. Schmahl

Peering Into the Eyes of Trilobites using EBSD C. Torney, M.R. Lee, and A.W. Owen

Texture and Anisotropy of MP35N Wire for Conduct Leads Bernard Q. Li and Tom Steigauf

Crystallographic Textures from the Exoskeleton of the Lobster Hornarus Arnericanus and Calculation of the Mechanical Properties of the Calcite Phase

L. Raue, H. Klein, D. Raabe, and H. Fabritius

TEXTURE EFFECTS ON DAMAGE ACCUMULATION

Experimental Characterization of the Effect of Crystallography on the Three Dimensional Nucleation and Growth of Fatigue Cracks in Metals

J-Y. Buffiere, E. Ferrie, H. Proudhon and W. Ludwig

Reversible Texture Transition during Accumulative Roll Bonding Naoya Kamikawa, Xiaoxu Huang, Grethe Winther, Nobuhiro Tsuji, and Niels Hansen

Evolution of Grain Boundary Microstructures in Molybdenum by Thermomechanical Processing from Single Crystals

Shigeaki Kobayashi, Sadahiro Tsurekawa, and Tadao Watanabe

569

577

587

595

605

61 9

627

637

657

669

681

Applications of Texture Analysis . xi

Local Characterization of Void Initiation on IF Steel by FIB-EBSD Technique

Orlando Leon-Garcia, Roumen Petrov, and Leo Kestens

Experimental and Simulation Study on Texture and Bendability of AA5XXX Aluminum Alloys

Y. Liu, Z. Long, X. Y . Wen, S. Ningileri, and S. K Das

Some Aspects on Grain Growth in ECAP Deformed and Heat Treated Aluminum 1.2% Hafnium Alloy

0. Al-Buhamad, M.Z. Quadir, and M. Ferry

Kinetic Measurements of Texture and Microstructural Evolution using Orientation Distribution Function and Residual Stress Relaxat ion

S. Saimoto, J. Cooley, and C. Gabryel

Texture and Micro-Hardness Evolution of Submicrograined Copper X. S. Yao, Y . D. Liu, Q. W. Jiang, X. Zhao, and L. Zuo

DIGITAL MICROSTRUCTURES

A Model of Plastic Spin Taking into Account Grain Interaction During Rolling

A. Fourty, J.W. Signorelli, and R.E. Bolmaro

CPFEM Investigation of the Effect of Grain Shape on the Planar Anisotropy and the Shear Banding of Textured Metal Sheets

Laurent Delannay, Maxime A. Melchior, Anand K. Kanjarla, Paul Van Houtte, and Javier W. Signorelli

Modelling of Primary Recrystallization using Digital Microstructures R.E. Loge, M. Bernacki, H. Resk, H. Digonnet, Y . Chastel, and T. Coupez

Two-Phase Microstructure Generation in 3D Based on 2D Sections of a Nickel Alloy

C.G. Roberts, S.L. Semiatin, and A.D. Rollett

Evolution of Local Damage Variable and Its Rate of Strain-Softening Material in Tension Based on Nonlocal Theory

X. B. Wang

Grain Interaction and Related Elastic Fields at Triple Junction in Low Deformed IF Steel: Micromechanical Model and Reconstruction from EBSD Orientation Data

A.A. Zisman, V.V. Rybin, M. Seefeldt, S. Van Boxel, and P. Van Houtte

693

70 1

709

71 7

725

735

745

757

771

779

787

xii . Applications of Texture Analysis

Gradient Matrix Method to Image Crystal Curvature with Discrete Orientation Data: Case Study of Triple Junction in Deformed IF Steel

803

A.A. Zisman, M. Seefeldt, S. Van Boxel, and P. Van Houtte

Author Index 81 5

Applications of Texture Analysis . xiii

Preface

It has been a pleasure, of a rather hard working type, to edit the proceedings for the 15th International Conference on Textures of Materials (ICOTOM 15). First and foremost I acknowledge the hard work and time that the symposium organizers have devoted to this task. This represents truly a community effort to sustain the development of this field of materials research.

Texture, or crystallographic orientation, plays an important role in many different areas of materials research and development. It grew out of metallurgical processing but now is significant to geology, welding, thin films, electronic devices, fuel cells, biomaterials and other applications too numerous to list. 1 am pleased that this meeting brings together such a broad range of interests. The papers included in this Ceramic Transactions volume (as well as its companion volume-Ceramic Transactions Volume 201, Applications of Texture Analysis) illustrate this broad range of applicability of the tools. Friction Stir Welding has undergone extensive development in recent years so it is appropriate that this volume has an entire section on the topic. Texture development and its effect on properties in steels remains of great interest to the community. Hexagonal metals such as titanium have greatly increased their range of applications so it is not surprising that texture is an essential aspect of these complex alloy systems. Magnetic fields have a strong effect on many materials and their influence on processing and resulting textures has attract- ed substantial interest. Lastly, materials design is being placed on a much firmer theoretical and computational foundation, as is evident in the work reported here. I have no doubt that the community will find these proceedings as essential in their work as they have for all the previous ICOTOM conferences.

I would like to thank the many colleagues who helped in organizing the conference and especially Dr. Carlos Tome of Los Alamos who put together the workshops that are such a distinctive feature of this conference. Many of these individu- als also made substantial contributions to the review process of the proceedings. Their names are listed on the Acknowledgments page.

I also thank the National Science Foundation, the Air Force Office of Scientific Research and the Alcoa Technical Center for their support of the conference. Their

xv

sponsorship made it possible for the many young scientists and engineers to attend the conference. The staff of The American Ceramic Society (ACerS) were unfail- ingly supportive and professional in their management of the conference. The Min- erals, Metals and Materials Society (TMS) also played an important role in devel- oping the workshops. I thank the many students and staff who contributed to the smoothing running and organization of the meeting.

A.D. TONY ROLLETT Carnegie Mellon University

xvi . Applications of Texture Analysis

Ac kn ow I ed g men t s

Conference proceedings co-editors

Brent Adams, Brigham Young University, USA

Katayun Barmak, Camegie Mellon University, USA

Thomas Bieler, Michigan State University, USA

Keith Bowman, Purdue University, USA

Paul Dawson, Come11 University, USA

Roger Doherty, Drexel University, USA

OlafEngler, Hydro Aluminium Deutschland GmbH and R&D Center, Germany

Hamid Garmestani, Georgia Institute of Technology, USA

Amit Goyal, Oak Ridge National Laboratory, USA

Erik Hilinski, US Steel, USA

Roland Loge, The Centre for Materials Forming, France

S. Lee Semiatin, Air Force Research Laboratory, USA

Robert Suter, Camegie Mellon University, USA

Carlos Tomt, Los Alamos National Laboratory, USA

Sven Vogel, Los Alamos National Laboratory, USA

Hasso Weiland, Alcoa Technical Center, USA

Stuart Wright, EDAX-TSL, USA

xvii

Thin Films (Microelectronics, HTSC)

THE TEXTURE OF THIN Nisi FILMS AND ITS EFFECT ON AGGLOMERATION

K. De Keyser. C. Detavernier , R. L. Van Meirhaeghe Department of Solid State Physics, Ghent University Krijslaan 28 1 S 1 Gent, 9000 Belgium

J. Jordan-Sweet. C. Lavoie IBM T.J. Watson Research Center Yorktown Heights New York, 10598 United States of America

ABSTRACT Nickel silicide films are used as contacting materials in the micro electronics industry. It

was recently [ I ] discovered that these films exhibit a peculiar type of texture, which was called ‘axiotaxy’, whereby certain lattice planes in the Nisi grains are preferentially aligned to (1 10)- type lattice planes in the single crystal Si substrate. In this contribution, we present a quantitative study of this phenomenon, using both XRD pole figure measurements and EBSD. Furthermore, we report a correlation between the texture of these Nisi films and their morphological stability during annealing at high temperature.

I n spite of the small grain size in these films, EBSD could be used to determine the volume fractions of the various texture components. This provided quantitative support for the claim that axiotaxy is the main texture component in these films, as about 40% of the grains belong to one of the axiotaxial texture components, and the remaining fraction exhibits a random orientation. A discussion of the techniques used during the measurement and analysis of the EBSD data is presented. as this must be given special consideration in view of the peculiar type of texture encountered in these films.

Secondly, both XRD and EBSD were performed after annealing the Nisi films at various temperatures and durations. It is known that thin Nisi films have a strong tendency to agglomerate 121. Our data indicates a correlation between the texture evolution and the agglomeration of the Nisi layer. Grains with axiotaxial orientation were observed to grow and thicken during the annealing process, by consuming neighboring randomly oriented grains. This suggests that the texture of the Nisi layer is a determining factor for the morphological stability of the film. The fact that grains with axiotaxial orientation grow during heat treatment can be related to the one dimensional periodicity at the interface, which lowers the interface energy and thus provides a driving force for the preferred growth of these grains. The agglomeration of Nisi films results in a significant increase of the sheet resistance. Therefore, these results illustrate the importance of texture control for the application of these films as contacts in micro-electronic devices.

INTRODUCTION Silicides play a vital role in the construction of micro-electronic devices [3]. They are

typically used as contacting materials on gate, source and drain regions in the CMOS process and

3

The Texture of Thin Nisi Films and its Effect on Agglomeration

also show promise in new applications such as fully silicided (FUSI) gates [4], and nano-wires [ 5 ] . Historically, three silicides have been used in micro-electronics as contacting materials, due to their low resistivity: initially, TiSi2 was used, but due to the difficulty of growing the low resistivity C54 phase of TiSil in narrow lines, the transition to CoSil was made. Further miniaturization lead to the adoption of Nisi as the currently used contacting material in deep submicron technology [3].

The viability of the use of a specific silicide depends on multiple parameters: it has to be possible to reliably grow the silicide in narrow lines. using a limited thermal budget (to insure compatibility with the other process steps), silicon consumption cannot be too high. and the silicide needs to stay stable and not degrade during all of the following process steps. The first and second problem could only be avoided by adopting Nisi as contacting material, however the third problem has been shown to be still significant. In contrast to CoSil and TiSiz. the Nisi phase is not the end-phase of the metal-silicon binary system (Nisi2 is), which, when further heating a Nisi contact in contact with the silicon substrate, could lead to a conversion of the contact to the higher resistivity Nisi2 phase, resulting in poor device performance. For thin Nisi layers, such as those typically used in the current deep submicron processes, it has been shown that this is only a secondary problem, as the thin Nisi film tends to break up and agglomerate first, long before it is converted into the Nisi2 phase [2]. As agglomeration leads to a huge increase in ,the resistivity of the contact, this has to be avoided. It has been shown that the addition of alloying elements to the Nisi layer can delay the agglomeration, however, the physical reason for this delay is not completely understood.

TEXTURE OF SlLlClDES Until recently, the texture of silicides was generally considered to be either random, or

epitaxial. Indeed, a lot of attention has been given to the effort of growing epitaxial silicides, such as CoSi2 and NiSi2, both cubic, which. due to the close matching of their lattice parameter to the cubic Si crystal lattice size, can be grown quite well epitaxially [6]. For the non-cubic phases, such as TiSi2 and Nisi, an epitaxial match between film and substrate is less obvious. Based on X-ray diffraction measurements in Bragg-Brentano geometry, it was concluded that these materials exhibit a random texture [7]. Indeed, lots of peaks, belonging to different planes, show up, indicating that not one single specific plane is parallel to the substrate. From this, one might jump to the conclusion that the film is thus randomly textured. However, looking at the intensities of the peaks indicates a discrepancy with the structure factors of the silicide. Measuring pole figures provided more information about texture. For CoSiz, this was done by Bulle-Lieuwma et al. [S], resulting in a variety of epitaxial orientations in which CoSiz can grow on Si 100. For Nisi. this resulted in the discovery of a new type of texture in thin films. which was given the name “axiotaxy” [l].

Texture of Nisi: axiotaxy An XRD pole figure for a 60nm Nisi film, recorded at the X20A beam line at the

National Synchrotron Light Source, can be seen in figure 1 a. Several arcs are visible, which can be explained by assuming that the grains making up the film have certain planes preferentially parallel to planes in the substrate. For Nisi, 4 sets of planes were identified as having a preferential orientation (table I). This alignment is called axiotaxy and results in an interface which is periodic along one direction, and axiotaxy can thus be considered as in-between random (no periodicity) and epitaxy (periodicity along multiple directions) In addition to the four

4 . Applications of Texture Analysis

The Texture of Thin Nis i Films and its Effect on Agglomeration

axiotaxies. several spots are visible. indicating the existence of an additional epitaxial component in the texture.

Figure 1: (202)+(211) pole figures of 60om Nisi films on Si 100. XRD (left, A) EBSD using GUSTAV (right, B)

The analysis of the texture of Nisi on Si (100). based on XRD pole figures. allowed the qualitative identification of the different texture components, however, getting quantitative information from these pole figures proves much more difficult. Pole figures can contain information from multiple planes if these planes have similar d-spacings, including planes from the substrate. and the very sharply defined features (i.e. axiotaxy) and low symmetry materials. make the use of standard ODF calculation tools impossible.

EBSD on Nisi To get an idea of the relative importance of the different axiotaxy components, electron

backscatter diffraction (EBSD) measurements were performed using an FEI Quanta 200F field emission SEM. Two types of measurements were carried out. A first type of scan was a typical EBSD map scan, where several points are collected in each of the grains, by using a step size which is considerably smaller than the grain size in the material. From these measurements, spatial information can be retrieved. such as grain boundaries or the location of grains with a specific orientation. For this measurement. the samples were first cleaned in a plasma oven in an A r - 0 2 n~ixture. to remove carbon contamination. Maps were then measured using step sizes of 2Onm and bigger. Only conclusions with limited reliability could be drawn from this data. Indeed, if one compares the statistics of the typical measurement techniques for texture in thin films. this problem becomes clear. Llsing XRD and a spot size of 1 mm2, recording a ole figure on a sample vAth an average grain size of about 100nm. results in infonnation from 10 grains. A !

Applications of Texture Analysis . 5

The Texture of Thin Nisi Films and its Effect on Agglomeration

typical EBSD map. using a step size of 2Onm, and a measurement grid of lOOOxl000 data points. gives information about only 10" grains. indicating that the statistics of this measurement are much worse than in the case of the XRD pole figures. This is confirmed when calculating pole figures from EBSD map measurements and comparing them to the XRD ones: the axiotaxy lines are hardly visible. A third technique. using TEM. results in even worse statistics. only a few grains can be investigated. For our goal of getting an overview of the texture, this was of limited use.

To improve the statistics in the case of the EBSD measurement. a second type of scan was devised, which we called an "EBSD pole figure scan". Here, a large grid is measured. using a large step size. As the step size is as big as, or bigger than the grain size in the film, each point is sampled in a different grain, resulting in orientation information for 1@1Oh grains. This strategy was carried out during multiple measurements on Nisi films of different thickness.

N i was sputter deposited on RCA cleaned and HF dipped Si 100 wafers, with a thickness of 45 and 30 nm. They were annealed at 550°C for 30 seconds. and then cooled down to room temperature. This results in the formation of either 90 or 60 nm of Nisi. Both traditional EBSD map measurements. as well as "pole figure measurements" consisting of 420 000 data points (EBSD patterns) with a step size of 250nm. were collected for each of the samples, using an HKL Channel 5 system. Pole figures were calculated from this data, using both the HKL software, as well as the GCJSTAV software, an in-house developed software package for texture analysis of both XRD and EBSD data. Figure 2a shows an EBSD map of the 60nm sample. The grains belonging to each of the texture components of table I were identified. They are indicated in color on figure 2b. Figure Ib shows the (202)+(21 I ) pole figure which was calculated from the EBSD data using the GUSTAV software. It has an evcellent resemblance to the XRD one shown i n figure la. It is worth noting that the excellent resemblance is only visible on the pole figures calculated using GCISTAV, as the fine curves, with relatively low intensity (total intensity of the axiotaxy is spread out along the line, while all the intensity of an epitaxial texture component contributes to a single point in the pole figure) easily gets lost in the coarse grid (pole figure is divided in cells with a size of multiple degrees in chi and phi) used by commercial ERSJ) software. which often has limited options to choose appropriate intensity scales too.

Figure 2: EBSD map on 60nm Nisi film. (a) shows band contrast, (b) shows texture components



Texture Component (21 1) axiotaxy (202) axiotaxy ( 1 03) axiotaxy ( 1 12) axiotaxy

Enitaxv

60nm Nisi 90nm Nisi ( I ) 90nm Nisi (2) 19 16 15 17 17 15 5 4 4 3 2 2 7 2 2

AGGLOMERATION OF THIN Nisi FILMS The integration of Nisi in the standard CMOS process faces an important problem: thin

films (< 50nm) of Nisi start to agglomerate at quite low temperatures (650°C). This phenomenon has been studied [2], and it has been shown that the addition of alloying elements can postpone this agglomeration to much higher temperatures [lo]. I n particular, the addition of Pt to a NiSi layer seeins to prevent this quite well [ 1 I]. A number of suggestions have been made regarding the mechanism by which Pt prevents this: a change in texture in NiPt,Si films compared to Nisi was reported. hinting at an effect of Pt on the texture, and calculations based on a phase-field model suggest that Pt moves to the grain boundaries of the Nisi film and prevents these boundaries from moving [ 121, however, the assumption in the latter model of random texture in the Nisi film is in our case clearly not valid.

Ni films with a thickness of 10 and 30 nm were sputter deposited on HI; cleaned Si 100 substrates. resulting in 20 and 6Onm Nis i films after annealing. The films with 30nm Ni received a 2nn1 Si cap. They were investigated using EBSD and XRD pole figures (X20A. NSLS). On the 20nm Nisi samples. EBSD proved impossible, due to the small grain size and thin films. XRD pole figures were successfully recorded on the 20nm Nisi samples. ramp annealed to either 500. 650. 700, 800 and 840°C. Figure 3 shows the evolution of the texture of the film in an ( 1 12) pole figure. All pole figures are plotted on the same, logarithmic, scale. For left to right (= increasing temperature) one sees a clear evolution in the texture of the film. At 700°C, the intensity in certain regions of the pole figures has significantly changed. and the axiotaxy lines increase in intensity. Further heating to 840°C results in a significant increase of intensity in the epitaxial spots, and a lower random background. Since an (hkl) type of axiotaxy reduces to a spot in an (hkl) pole figure. the number of XRD counts in this spot is proportional to the amount of material having the axiotaxial orientation. and can be used to get an estimate of the importance of a specific axiotaxy texture component. However, for the (202). (21 I) and ( 1 12) axiotaxy, the d- spacing of those Nisi planes is close to the one of the Si (220) plane. making it impossible to isolate the XRD signal of Nisi from the Si (220) signal, since they both result in spots at the


From the EBSD measurements. volume fractions for all of the texture components could be calculated [9], the results for which can be found in table 11. It is important to stress that the absolute numbers for the volume fractions based on EBSD. when carried out on materials with small grains and low symmetry, have a limited reliability, as the software used to analyze these EBSD patterns tends to introduce errors, especially on lower symmetry materials like Nisi (orthorhombic). Furthermore, there is a slight dependence of the volume fraction on the settings of the microscope. such as acceleration voltage and spot size. Still. the numbers confirm that axiotaxy is an important part (about 40%) of the texture of the thin Nisi films, however it also shows that randomly oriented grains make up an important part of the film as well.


same location in the pole figure. For Nisi (103). this problem does not occur. and figure 4 shows the X-ray intensity. corrected for background, in the (103) fiber axis, as a function of annealing temperature. The intensity stays constant up until 650°C after which a sharp increase is visible. If one compares this to the resistance measurements in reference [2]. this can be correlated to the sharp increme in sheet resistance of Nisi films between 650 - 700°C. We can conclude that the increase of' the resistance is mostly likely related to the change in texture of the material. Combining the information from figure 3 and 4, this suggests that the random oriented grains will disappear during agglomeration. in favor of epitaxial and axiotaxial grains.

Figure 3: XRD (112) pole figures on 2Onm Nisi films at different temperatues

I

I

Figure 4: X-ray intensity for (103) axiotaxy as function of annealing temperature

As EBSD measurements on the 20nm Nisi samples were impossible. we also looked at the thicker 60nm Nisi layers. Due to their increased thickness, agglomeration will be much more difficult, and the layer will first convert to Nisi2 when heating to higher temperatures (700°C). To prevent the Nisiz growth, the 60nm Nisi layers were annealed at a lower temperature. 550OC. for different time periods. Agglomeration proved to be very slow, and even after a 72h anneal. the films were only starting to agglomerate. On the samples, EBSD measurements were carried out using 200000 data points, always using identical settings, both in hardware and software (Channel 5, Advanced Indexing). The volume fractions for each of' the axiotaxy texture components were calculated. both for the sample spike annealed to 550°C with no dwell time. as



Texture Component (21 1 ) axiotaxy (2O~axiotaxy (1 0 3 ) axiotaxy (1 12) axiotaxy total axiotaxy

for a sample with a dwell time of 72h at 550°C. In table 111, the volume fractions are indicated. Even though agglomeration has only started. we can already notice an increase in the volume fractions for the axiotaxial grains for 24% to 30%. supporting the results on the 2Onm Nisi samples. The difference in the absolute values for the volume fractions with table 1 are most likely caused by the addition of a 2nni Si cap, to prevent the Ni from oxidizing. XRD pole figures were recorded as well (tigure 5). Plotted on the same scale. the increase ofthe axiotaxial and epitaxial components after a 72h anneal is clearly visihle.

O h dwell time 72h dwell time 9 1 1

12 10 3.5 5.5 1.5 1.5 24 30

______


Mechanism for agglomeration Since epitaxial grains have an excellent interface match with the substrate. and axiotaxial

grains. while slightly worse than epitaxy. still have a decent interface match due to the 1- dimensional periodicity. there is a driving force for axiotaxial and epitavial grains to consunie randomly oriented neighbor grains. due to the lowering of the interface energq which can be accomplished in that way. As noted in [I] . the axiotaxial orientation relation has the property of being largely independent of the shape of the interface. Going from a flat interface to a spherical one results in the louest amount of interface energy per unit of volume of the grain. By consuming random grains and curving the interface, axiotaxial grains both reduce the interface energy per unit of surface (going from zero- to one-dimensional periodicity at the interface). as well as the total surface at the interface (due to the curving ofthis interface). This was confirmed by TEM measurements in [2], were axiotaxy grains are shown to have a ciwed interface in agglomerated films. For epitaxial grains. the typical plane-on-plane matching depends heavily on the shape ofthe interface with the substrate. Curving results in a loss of the low energy epitaxial

Figure 5: (1 12) pole figures on 60nm Nisi films, spike annealed to 55WC with a dwell time ofOh (left) or 72h (right).

Table 111: volume fractions (in %) fmm EBSD measurements on 60nm Nisi films, ramp annealed tn T T W r with I( rlu-ell time nf nh nr 7Zh


interface, thus the epitaxial grains can only increase their size by growing laterally, and keeping the interface plane flat. As agglomeration is in fact nothing more than a thickening and curving of grains, the occurrence of axiotaxial grains will thus promote the agglomeration.

From the pole figures in [lo, 1 I] , it is clear that adding alloying elements changes the texture of the material, by suppressing the axiotaxial grains and promoting the epitaxial ones. In light of our results, it becomes evident why this delays agglomeration.

CONCLUSION We have shown the possibility of investigating the texture of silicides using EBSD,

resulting in information on volume fractions for the different texture components. Using XRD pole figures and EBSD, we have studied the evolution of the texture in thin Nisi films during agglomeration and have found evidence for a correlation between axiotaxy and tendency to agglomerate. From these results, we were able to explain the effect of alloying elements on the agglomeration behavior.

REFERENCES I C. Detavernier, A. S. Ozcan, J. Jordan-Sweet, E.A. Stach, J . Tersoff, F.M. Ross, C.

Lavoie, "An off-normal fibre-like texture in thin films on single-crystal substrates." Nature 426,

' D. Deduytsche. C. Detavemier, R.L. Van Meirhaeghe, C. Lavoie, "High-temperature degradation of Nisi films: Agglomeration versus Nisi2 nucleation." J. Appl. Phys. 98(3), 033526

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Future Trends", Crit. Rev. Solidstate Mater. Sci., 28(1), 1-129 (2003) J.A. Kittl, M. A. Pawlak, et al, "Transient and end silicide phase formation in thin film

Ni/polycrystalline-Si reactions for fully silicided gate applications." Appl. Phys. Lett. 91( 17). 1 72 108 (2007)

C.A. Decker, R. Solanki, J.L. Freeouf, J. Carruthers, D.R. Evans, "Directed growth of nickel silicide nanowires." Appl. Phyx Lett. 84(8), 1389-1 391 (2004)

' L.J. Chen, J. W. Mayer, K.N. Tu, "Formation and structure of epitaxial Nisi2 and CoSi2". Thin Solid Films, 93, 135-141 (1982)

' F. Dheurle, C. S. Petersson, J.E.E. Baglin, S.J. Laplaca, C.Y. Wong, "Formation of thin films of Nisi - Metastable structure, diffusion mechanisms in intermetallic compounds", J. Appl.

' C. W. T. Bullelieuwma, A. H. Vanommen, J. Homstra, C. Aussems, "Observation and analysis of epitaxial growth of CoSiz on (1 00) Si", J. Appl. Phys. , 7 1 (5), 22 1 1-2224 (1 992)

K. De Keyser, C. Detavernier, R.L. Van Meirhaeghe, "Characterization of the texture of silicide films using electron backscattered diffraction", Appl. Phys. Lett., 90( 12), 121 920 (2007)

D. Deduytsche, C. Detavemier, R.L. Van Meirhaeghe, J.L. Jordan-Sweet, C. Lavoie, "Formation and morphological stability of Nisi in the presence of W, Ti, and Ta alloying elements." ./. Appl. Phys. lOl(4) 044508 (2007)

I ' C. Detavemier. C. Lavoie, "Influence of Pt addition on the texture ofNiSi on Si(OOI).", Appl. Ph s Lett., 84(18). 3549-3551 (2004)

I'M. Bouville, S. Y. Hu, L.Q. Chen, D.Z. Chi, D.J. Srolovitz, "Phase-field model for grain boundary grooving in multi-component thin films.", Modell. Simul. Muter. Sci. Eng., 14(3),

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Applications of Texture Analysisdownload.e-bookshelf.de/download/0000/5728/33/L-G-0000572833... · The Texture of Thin Nisi Films and Its Effect on Agglomeration . 3 . K. De Keyser,