Recrystallization Edited by Krzysztof Sztwiertnia RECRYSTALLIZATION Edited by Krzysztof Sztwiertnia INTECHOPEN.COM Recrystallization http://dx.doi.org/10.5772/2028 Edited by Krzysztof Sztwiertnia Contributors Yuriy Perlovich, Margarita Isaenkova, Guanghui Li, Tao Jiang, Yuanbo Zhang, Zhaokun Tang, Su-Hyeon Kim, Dong Nyung Lee, Pingguang Xu, Yo Tomota, Yousef Javadzadeh, Sanaz Hamedeyazdan, Solmaz Esnaashari, Krzysztof Maciej Sztwiertnia, Magdalena Bieda-Niemiec, Anna Korneva, Ichiko Shimizu, Valerie Dupray, Renu Chadha, Poonam Arora, Anupam Saini, Swati Bhandari, Kazimierz Ducki, Kinga Rodak, Rimma Lvovna Brodskaya, Ioan Coriolan Balintoni, Ramin Ebrahimi, Ehsan Shafiei, Vadim Glebovsky, Fritz Appel, Kumkum Banerjee, Lisandro Pavie Cardoso, Livio Amaral, Eliermes Meneses, Adenilson Dos Santos, Rossano Lang, Alan De Menezes, Shay Reboh, Toni Mattila, Jorma Kivilahti © The Editor(s) and the Author(s) 2012 The moral rights of the and the author(s) have been asserted. 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ISBN 978-953-51-0122-2 eBook (PDF) ISBN 978-953-51-6131-8 Selection of our books indexed in the Book Citation Index in Web of Science™ Core Collection (BKCI) Interested in publishing with us? Contact book.department@intechopen.com Numbers displayed above are based on latest data collected. For more information visit www.intechopen.com 4,100+ Open access books available 151 Countries delivered to 12.2% Contributors from top 500 universities Our authors are among the Top 1% most cited scientists 116,000+ International authors and editors 120M+ Downloads We are IntechOpen, the world’s leading publisher of Open Access books Built by scientists, for scientists Meet the editor Krzysztof Sztwiertnia is a professor at the Institute of Metallurgy and Materials Science, Polish Academy of Sciences (IMMS PAS). He graduated at the Academy of Mining and Metallurgy in Krakow, Poland. After graduation, he worked successively in the IMMS PAS, the Institut für Werkstoffe der Technischen Universität Braunschweig, in Germany, and again in the IMMS PAS. His research interests span various areas of crystallographic orientation-re- lated investigations. In particular, he is interested in deformation and recrystallization processes in metals, as well as methods of measurement, description and analysis of texture, and microstructure of polycrystalline materials. Professor K. Sztwiertnia is an author and co-author of over 100 research papers and two monographs. Contents Preface X III Part 1 Recrystallization of Metallic Materials 1 Chapter 1 Development of Texture and Substructure Inhomogeneity by Recrystallization of Rolled Zr-Based Alloys 3 Yuriy Perlovich and Margarita Isaenkova Chapter 2 Recrystallization of Dispersion-Strengthened Copper Alloys 23 Su-Hyeon Kim and Dong Nyung Lee Chapter 3 Application of Orientation Mapping in TEM and SEM for Study of Microstructural Evolution During Annealing – Example: Aluminum Alloy with Bimodal Particle Distribution 43 K. Sztwiertnia, M. Bieda and A. Kornewa Chapter 4 Crystal Growth: Substructure and Recrystallization 59 Vadim Glebovsky Chapter 5 Recrystallization Behavior During Warm Compression of Martensite Steels 87 Pingguang Xu and Yo Tomota Chapter 6 The Deformability and Microstructural Aspects of Recrystallization Process in Hot-Deformed Fe-Ni Superalloy 109 Kazimierz J. Ducki Chapter 7 Physical Metallurgy and Drawability of Extra Deep Drawing and Interstitial Free Steels 137 Kumkum Banerjee X Contents Chapter 8 The Failure Mechanism of Recrystallization – Assisted Cracking of Solder Interconnections 179 Toni T. Mattila and Jorma K. Kivilahti Chapter 9 Mathematical Modeling of Single Peak Dynamic Recrystallization Flow Stress Curves in Metallic Alloys 207 R. Ebrahimi and E. Shafiei Chapter 10 Phase Transformations and Recrystallization Processes During Synthesis, Processing and Service of TiAl Alloys 225 Fritz Appel Chapter 11 The Effect of Strain Path on the Microstructure and Mechanical Properties in Cu Processed by COT Method 267 Kinga Rodak Part 2 Recrystallization of Minerals 301 Chapter 12 Zircon Recrystallization History as a Function of the U-Content and Its Geochronologic Implications: Empirical Facts on Zircons from Romanian Carpathians and Dobrogea 303 Ioan Coriolan Balintoni and Constantin Balica Chapter 13 Recrystallization of Fe 2 O 3 During the Induration of Iron Ore Oxidation Pellets 329 Guanghui Li, Tao Jiang, Yuanbo Zhang and Zhaokun Tang Chapter 14 Ion-Beam-Induced Epitaxial Recrystallization Method and Its Recent Applications 351 Rossano Lang, Alan de Menezes, Adenilson dos Santos, Shay Reboh, Eliermes Meneses, Livio Amaral and Lisandro Cardoso Chapter 15 Steady-State Grain Size in Dynamic Recrystallization of Minerals 371 Ichiko Shimizu Chapter 16 Recrystallization: A Stage of Rock Formation and Development 387 R.L. Brodskaya and Yu B. Marin Part 3 Recrystallization in Pharmacology 401 Chapter 17 Recrystallization of Enantiomers from Conglomerates 403 Valérie Dupray Contents X I Chapter 18 Recrystallization of Drugs: Significance on Pharmaceutical Processing 425 Yousef Javadzadeh, Sanaz Hamedeyazdan and Solmaz Asnaashari Chapter 19 Crystal Forms of Anti-HIV Drugs: Role of Recrystallization 447 Renu Chadha, Poonam Arora, Anupam Saini and Swati Bhandari Preface Recrystallization and related phenomena that occur during thermomechanical processing of all types of crystalline materials are areas of intensive research. However, particular subject matters of research differ depending on scientific discipline. In geology, recrystallization is a process that occurs during natural deformation of rocks and minerals subjected to high temperature and pressure. Grains, atoms or molecules can be packed closer together. Under the influence of these metamorphic processes, new mineral grains can be created in crystalline form. Analysis of the consequences of these processes is often used for quantification in geochronology. In chemistry and other closely related fields such aspharmacology, recrystallization is often applied as a procedure for purifying compounds. In metallic materials, recrystallization and related annealing phenomena have been long ago recognized as technologically important and scientifically interesting. Perhaps for this reason, they have been studied most widely. Metallurgical research in this field is mainly driven by requirements of industry. Significant progress has been made ,expressed in hundreds of publications, reviews and monographs. However there are still considerable gaps in understanding of the recrystallization processes. Lack of a complete explanation can be attributed to high complexities of the phenomenon, which consists of a superposition of the processes of local nucleation and grain growth. These processes depend strongly on the characteristics of the matrix, that is usually complex and heterogeneously deformed. Quantitative characterization of the deformed state and description of grain boundary properties constitute the areas of fundamental importance for the understanding of recrystallization. Comprehension of the nature of the deformed state as the precursor of recrystallization and the nature of local instabilities in the heterogeneous matrix can be achieved by the techniques of Orientation Imaging Microscopy (OIM), both in scanning and transmission electron microscopes (SEM and TEM). However, the standard techniques of Electron Backscatter Diffraction (EBSD) in SEM - although very X Preface useful for testing of advanced recrystallization stages ,proved to be less useful when a high spatial resolution in orientation measurement is required. In order to obtain a better spatial and angular resolution, similar techniques developed for the TEM can be used. The TEM offers spatial resolution an order of magnitude better than these in SEM and it can be used for quantitative nanoscale analysis of the microstructure at the beginning of the process. It is also essential to note the importance of dynamic studies in the SEM and in the TEM that should be capable of providing information about temporal relationships between changes occurring in a material throughout the course of recrystallization. For the above reasons, we have included in one of the chapters an example of an application of OIM/TEM to analyze early recrystallization stages. The entire book should be seen as a snapshot of the subject at this particular moment in time, as seen by scientists, who work on recrystallization-related issues from wide ranging perspective of scientific disciplines, from geology to metallurgy. The authors wish to emphasize that the progress in the particular field of materials science has been possible today thanks to coordinated action of many research groups that work in materials science, chemistry, physics, geology and other sciences. Thus, it is possible to perform a comprehensive analysis of the scientific problem.The analysis starts from the selection of appropriate techniques and methods of characterization. It is then combined with the development of new tools in diagnostics, and it ends with modeling of phenomena. The book shows selected results obtained during the last years. Its main topics are recrystallization of metallic materials, recrystallization of minerals and recrystallization in pharmacology.They are grouped in the appropriate sections. Each section is illustrated with problems or applications of the process. For example, chapter 1 in section 1 is focused on recrystallization of Zr-based alloys, and second chapter in section 3 on recrystallization of drugs. Prof. Krzysztof Sztwiertnia Institute of Metallurgy and Materials Science, Polish Academy of Sciences, Krakow, Poland Part 1 Recrystallization of Metallic Materials 1 Development of Texture and Substructure Inhomogeneity by Recrystallization of Rolled Zr-Based Alloys Yuriy Perlovich and Margarita Isaenkova National Research Nuclear University “MEPhI” Russia 1. Introduction Recrystallization of α -Zr is of the great interest both as a rather complicated scientific phenomenon and as a process of the practical importance for applications in the nuclear industry. Meanwhile in the most known monographs on Zr and Zr-based commercial alloys (Douglass, 1971; Tenckhoff, 1988; Zaymovskiy et al., 1994) the recrystallization of α -Zr is considered on the basis of experimental data, obtained more, than 40 years ago. These data urgently require corrections with taking into account the up-to-day theoretical conceptions and the continuous progress in experimental technique. Zr-based alloys are characterized by α↔β phase transformations within the technologically important temperature interval 610°- 850°C and by operation of various mechanisms of α -Zr plastic deformation, including slip by basal, prismatic and pyramidal planes as well as twinning in several systems. These features are responsible for very complicated distribution of strain hardening and the corresponding tendency to recrystallization in products from Zr-based alloys. The given chapter makes up some gaps in our knowledge concerning different aspects of recrystallization as applied to α -Zr. 2. Regularities of recrystallization in sheets and tubes of Zr-based alloys with multicomponent rolling textures The most widespread data on recrystallization regularities in α -Zr pertain to sheets and tubes with the final stable rolling texture of α -Zr (0001)±20°-40° ND-TD <10 1 � 0> (Douglass, 1971), where ND – normal direction and TD – transverse direction. Meanwhile later the new detailed data were obtained concerning texture development in α -Zr under rolling. In particular, it was established that by rolling of a textureless slab the intermediate texture (0001) ±15°-25° ND-RD <11 2 � L> forms, where RD – rolling direction, and keeps its stability up to the deformation degree of 70%, whereupon it converts to the final stable texture (Isaenkova & Perlovich, 1987a, 1987b). Main components of these textures in the order of formation were denoted as T1 and T2. Besides, components (0001)<10 1 � 0> (T0) and {11 2 � 0}<10 1 � 0> (T3) are present often in textures of rolled sheets and, especially, tubes. All these texture components form owing to activity of concrete combinations of plastic deformation mechanisms, have their characteristic strain hardening and therefore show Recrystallization 4 different tendencies to recrystallization. In the real case of a multicomponent texture the development of recrystallization must be additionally complicated by interaction between different components in regions of their contact. Indeed, according to (Isaenkova et al., 1988; Perlovich et al., 1989), resulting changes of α -Zr rolling textures in the course of recrystallization can not be reduced to 30°-rotation around basal normals and require for more complex description. In order to investigate this question in more details, the following work was undertaken. 2.1 Materials and methods Recrystallization was investigated in sheet samples of alloys Zr-2,5%Nb, Zr-2,3%Cr and pure Zr as well as in tube samples of the alloy Zr-2,5%Nb. Sheets were produced by longitudinal or transverse cold rolling up to deformation degrees in the range from 40% to 90% in such a way as to form the following textures: T1, T1+T2, T2, T1+T2+T3. The weak component T0 was present everywhere. Perfection parameters and mutual relationship of different components varied. The channel tube was cold-rolled by 50%- thinning of its wall. All samples were annealed in dynamic vacuum at temperatures 500°- 600°C during 1-5 h. The main used method was X-ray diffractometric texture analysis. Direct pole figures (PF) (0001), {11 2 � 0} and {10 1 � 2} were measured by the standard procedure (Borodkina & Spector, 1981). To reveal PF regions, where texture changes by recrystallization are predominantly localized, diagrams of PFs subtraction (SD) were calculated and constructed. SD involves contours of pole density equal changes, having been drawn by comparison of recrystallization and rolling textures. In addition, PF sections of interest were constructed to follow redistribution of basal and prismatic normals in the course of recrystallization. 2.2 Recrystallization in sheets Analysis of PFs {11 2 � 0} shows that texture changes by recrystallization can be described as rotation around the motionless basal axis only in the case of the rolling texture consisting largely of the component T2. However, the angle of such rotation varies: e.g. in the case of cold rolling by 60% for pure Zr recrystallized at 500°C this angle is equal to 30°, while for the alloy Zr-2,5%Nb recrystallized at 580°C – only 20°. When the rolling texture consists predominantly of the component T1, recrystallization does not involve lattice rotation around basal normals, - this is confirmed by invariance of PF{10 1 � 2}. Main results concern reorientation of basal normals by α -Zr recrystallization, i.e. changes of PF(0001). Superposition of SD and PF(0001) is shown in Fig. 1 for the sheet alloy Zr-2,5%Nb rolled up to deformation degrees 40, 60 and 80%, corresponding to formation of different textures: T1, T1+T2, T2. The densest cross-hatching indicates zones, where texture are localized predominantly. These zones are situated at slopes of initial texture maxima, increasing scattering of the recrystallization texture. Hence, the model of inhomogeneous strain hardening, proposed in (Perlovich, 1994) for textured BCC-metals, is true for HCP α - phase also. But while taking into account the multicomponent character of observed rolling textures, regularities of recrystallization should be more complicated.