5 IWWW”MINIMUM”!!!WWWHIWHIIHIIHI 972 '—I :1: m s {433319 This is to certify that the thesis entitled A STUDY OF ROLLING AND RECRYSTALLIZATION TEXTURES IN Cu - 5 % Aq presented by Wonjoonq Kim has been accepted towards fulfillment of the requirements for m.s _ materials science degree in QMajor profego: 21/2/[gg 0-7639 MS U is an Affirmative Action/Equal Opportunity Institution Date MSU LIBRARIES “ RETURNING MATERIALS: Place in book drop to remove this checkout from your record. ‘FINES will be charged if book is returned after the date stamped below. A STUDY OF ROLLING AND RECRYSTALLIZATION TEXTURES IN CU--S%Ag 8v Wonjoong Kim A DISSERTATION Submitted T0 MICHIGAN STATE UNIVERSITY in partial fquiIment of the requirements for the degree 01’ MASTER OF SCIENCE Department of I’letaIIurgy, Mechanics and MateriaIs Scienc I986 ABSTRACT A STUDY OF ROLLING AND RECRYSTALLIZATION TEXTURES IN Cu-SifiAg By Wonjoong Kim The rolling and recrystallization texture of Cu-SzAg were obtained from both ( I I I ) and (200) reflections by using the Schuoz refoection method. Complete pole figures were then obtained by normaling all data with respect to the random powder specimen. For the roIIing textures the transition observed for both the Cu—SiEAg solid solutionalloy and the two phase alloy is similar to that observed in the brass and Cu-P alloy. For the recrystallization textures, however, both the Cu-Ag solid solution alloy and the Cu-Ag two phase alloy didn't show brass recrystallization textures. While the recrystallization textures of the Cu—Ag solid solution annealed at 60000 revealed a pass component in addition to the cube— and {258}< I 2 I > component present at 5500C the recrystallization textures of the Cu—Ag two phase alloy were composed of the 9035- and {258}<121 > component. ACKNOWLEDGEMENTS I would Iike to express my deep sense of gratitude to Professor Gunter Gottstein for his constasnt guidance and encouragement during the course of this research. I would also like to thank my colleagues Dongteak Chung, Chulsoo Kim, and Wookwhan Sur for their help and encouragement all through this project. I extend special thanks to my family for their encouragement during my period of study. Finally I would like to thank the Department of Energy for providing the fund for this research. iii Chapter 4.I 4.l.l 4.I.2 4.2 4.2.1 TABLE OF CONTENTS P698 LIST OF FIGURES ....................... iv INTRODUCTION .......................... I REVIEW OF PREVIOUS STUDY . . ............. . . 2 Rolling Textues of fee Metals and Alloys ................ 2 Theories of Rolling Texture Transition ................. 8 Annealing Textures of Icc Metals and Alloys . . . . ........... 12 Theories of the Development of Recrystallization Texture ......... IS EXPERIMENTAL PROCEDURE AND TECHNIQUES ............. l8 Pole Figure System . . . . .................... I8 Principles of X-ray Texture Goniometers . . ............ 18 POIe Figure Projections . . ................... I9 Installation of Pole Figure System . . . ............... 2i Software System ...... . ........... . . . . 24 Operation of System . ............... 28 Specimen Preparation . ...... 29 Rolling Process of Cu-S%Ag . ............. 29 Heat Treatment of the samples . ........ 32 RESULTS AND DISCUSSION . ............. 34 Rolling Texture . .............. 34 Experimental Results . ........... 34 Discussion ..... 34 Recrystallization Texture . ...... 38 Experimental Results . ..... 35 4.2. 8 Discussion . Summary and Conclusions . 35 . 42 LIST OF FIGURES Figure No. EEG} f\.) (N Positions of the < I I I > ,< I 00> poles of some components of the texture . . . A . . . . . . , . . . . . . . . . . . . . 3 ( I I I ) pole figures for Cu anda-brass after roIIing at rccm temperature..._.................. 7 ( I I I) pole figures obtained for Cu after rolling at different temperatures......................7 Shear misfit produced by the three different shear components (a) Taylor case.(b)misfit in exz.(c)misfit in exyand (d) misfit lf‘IEyz . Orientation distribution along the skeleton line as calculated for {I I I} <1 10> slip according to the theory of relaxed constraints if (a) 6X2 (b) exy (c) Eyz ((1) 6X2 and exy (e) all shear strainsareassumedt00eunconstrained . . . . . . . , . i . . IO ( I I I ) pole figures of a a ~brass single crystal after unconstrained rolling (a) and after rolling with constraints on Eyz (B). which leads to twinning on that I I I ) plane perpendicular to ID (b) Schematic of the shape change of the initially rectangular rolling plane of the crystal. (c) too as a function of the thickness reduction for the cases of I6 Pole figure system configuration. . I7 ( I I I ) pole figures of a lithium fluoride single crystal and an aluminum single crystal..................._........26 I8 Pole figuresoftwaresystem configuration ..... . . . .. . . . 27 I9 Hardnessvariationduringannealingofrolledspecimens. . . . . . . 33 20 ( I I I),(200) pole figures for Cu-S%Ag (solid solution) rolled to 95% reduction at room temperature. . . . . _ .. . . . . . . . .. . 37 2I ( I I I),(200) pole figures for Cu-Sf‘EAg (two phase alloy) rolled to 95% reductionatroom temperature. . . . . . . . . . . . . . . . .. 38 22-I ( I I I),(200) pole figures of recrystallization textures of Cu-SiBAg solid solutionalloyafter rollingandannealingat8500C. . . . . . . . . 39 22-2 ( I l I),(200) pole figures of recrystallization textures of Cu-SRAg solid solutionalloyafter rollingandannealingat600°C. . . . _ . . _ .40 23 ( I I I).( 200) pole figures of recrystallization textures of Cu-SiEAg two phase alloy after rolling and annealing at 8000C . . . . , . 41 vii unconstrained(a)andconstrained(Gldeformation . . . . . . II 7 ( I l l ) pole figures of rolling textures of Cu-Zn alloys before and after recrystallization. (a),(c),and (e) subsequent to rolling with 95% thickness reduction of (a)Cu andtc)Cu-S%Zn at room temperature and (e) Cu—SiK Zn at 770K. (b) .( d), and (f) show the corresponding textures after primary recrystallization. . 8 400 rotations of both components of the (GI I )I2 I I] orientation. I0 A sheet sample mounted in back-reflection position. I I Starting position of the sample. I 2 The diffraction vector dis brought into the sample direction {a,B} by the rotations d) and t0 1. IS Geometric illistration of aXial motion. I4 The illustration of pole figure projection. IS The two dimensmnal illustration of pole figure protection. viii 20 20 22 22 .23 CHAPTER I INTRODUCTION The rolling textures as well as the recrystallization textures in fee alloys as function of the composition has been the subject of several investigations,( I ). Most of these investigations are based on the analysis of pole figures. This method led to an approximation of the rolling textures by the three ideal orientations {OI I} <2I I>, {I23} <634>, and {I I2} in the case of pure copper and by the two orientations {OI I } <2I I } and {OI I } < IOO> in the case of a. brass with high Zn-content. After primary recrystallization, in the first case the cube orientation and in the second case the brass redrystallization orientation was observed.( I ). For the intermediate Zn-content the rolling textues were found to give a continuous transition from one to the other. For the corresponding recrystallization texture, however, discontinuous. much more complicated transition was found with several components to newly occur and to disapper which seemed to be qualitatively different for different alloy systems. Thus, in the present paper a qualitative investigation of the variations of the rolling and recrystallization textures in Cu—SiKAg alloy was carried out by determining pole figures. For the rolling and annealing textures two kinds of sample were used. The first was used to study the rolling and annealing texture development of a supersaturated solid solution which was annealed at 90000 for 7 hours,followed by water quenching. Also in order to study the effect of annealing temperature to the recrystallization textures one of the solid solution sample was annealed at 5500C and the other was annealed at 6000C. The second was designed to investigate the rolling and annealing texture development of the two phase material (a solid solution + [3 solid solution) and accomplished by annealing at 6000C for three hours and then cooled by water quenching CHAPTER 2 REVIEW OF PREVIOUS STUDIES Quantative methods for pole figure measurement have been widely studied during the past thirty years. In this review an attempt is made to summarize the basic of this studies under the same heading. 2. I Rolling Textures of FCC Metals and Alloys There are two types of rolling textures. One is expressed as copper type texture and the other is the brass type texture . The copper type texture occurs in metals of high stacking fault energy and high deformation temperatures, while the brass type texture exists in metals of low stacking fault energy at low deformations. Textures in rolled sheet can be usually described by a fe ideal orientations in terms of the plane (hkl) that lies parallel to the plane of the sheet and the direction [uvw] that is parallel to the rolling direction. Some typical ideal orientations are shown in Figure I. The copper type rolling texture can be expressed as{ I 12}. { I23}<634>, andTOI I}<21 I> components whilethe brass type texture is characterized by { I IO} plus {I IO} <00 I > component. A number of parameters have been suggested to characterize the fcc rolling texture transition,Figuer 2. A transition from the copper type to the brass type texure which occurs on alloying has been found with decreasing deformation temperature and decreasing stacking fault energy. In case of copper alloys (2) this transition can be inferred by decreasing the temperature of rolling or by increasing of the solute content (I,e, Zn) at constant rolling temperatureas shown in Figure 3. An increasing tendency for mechanical twinning during deformation Is the mechanism which causes the ice rolling texture transition with decreasing IDEAL ORIENTATION /./ x... AAAAAAAAAAAAAAAAAAAA / \ Polling component / . \\ Ctl'POSlI-lon /’ \ K“ i \, / ROLLING DIRECTION \ - + I I I \ / \ . ROLLING ILMIE I2IOTIIIAL IDEAL ORIENTATION ,r" \. AAAAAAAAAAAAAAAAAAAA - . /’ \ Polling Component / \ Cit-position / \ ROLLING PLillIE IIORIIAL - I l 2 \\ / IIOLLIIIG DIRECTION \ ' ~ I I I \ / ‘\ “9'1”: I ’ I . Positions. of the . I I I>,<200> poles of Cu- component of the texture innit ORIENTATION ,er ~:~\ I‘.I'x.A.;'-.1‘.Af\/\AAAAAAAAAAAA / ‘\ Rolling component / \ Its-post tion /’ mount: PLANE IIORIIAL - o I I \\ ROLLING DIRECTION ‘\ — 2 i I \ / \ . IDEAL ORIENIRIION f!" T’\ AAAAAAAAAAAAAAAAAAAA ,, ‘\ u \ Rolling Component / \ . . / Bs-poSIIIon /’ \ .0. ROLLING Punt IIORIIAL e I 1 \ / ROLLING DIRECTION \ ' - 2 I I / F ldure I—z : PFIRIIIUTIS iii the. < I I I>. poles of BS-comoonent of the. texture IDEAL ORIENTATION / ~.\ AAAAAAAAAAAAAAAAAAAA / \ recr. component /# m\ EIOSS / 8 \ l ROLLING PLANE NORMAL \ - .t- o I I \.\ // ROLLING DIRECTION ‘\ z" s- I o o \ / \. f/ \-.\ —” . LR If I/IT-F- . mnxxx\_ IINIWIINIIIIIII /” \x // \\ recp. component // \\ ,/ ‘\ 9055 // \ ROLLING PLANE NORMAL \ + it I I \\ / ROLLING DIRECTION ‘\ " + I o o \ / \. //' \‘x‘ __.r “KW!” Figure I 3 ' positions of the < I I It, <200> poles of goss- component of the texture. IDEi‘iL ORIENTATION if“ “X AAAAAAAAAAAAAAAAAAAA // \\ recr. component / \ "Rs-position / . \ ROLLING PLANE IIOIIIIAL . L o I 1 \. / ROLLING DIRECTION \ T ? 3 3 \\. ///// \. innit. ORIENTATION ff” \ AAAAAAAAAAAAAAAAAAAA / \ I’E’Cl". component / \\ ”B's-position / \ i i ROLLING PLANE IIORIIAL '* II I I \.\ II/ ROLLING DIRECTION \ — i 3 3 \ "o I ‘x... EM Figure I ~ 4 piiis'iiitiris I'IT lhe <1 I I >. (200,» poles of TBS‘COIIIDOrienl OI the texture Figure 2: ( I I I ) pole figures for Cu anda—brass after rolling at room tem perature. Figure 3' t I I I ) pole. figures obtained for Cu after rolling at different temperatures. stacking fault energy,( 3). Thus the copper-brass texture transition Is mainly attributed to the formation of deformation twin. 2.2 Thories of Rolling Texture Transition The rolling texture is formed in the course of shear deformation under the action of oriented external forces. The condition of deformation, the operative slip systems, and the behaviourof dislocations in the given material have a pronounced effect on deformation textures. The deformation structure of heavily rolled fcc materials is characterized by elongated subgrains. Theoretical treatments of volling texture development are based on the Sachs or the Taylor principle. The Sachs model assumes that every grain of a polycrystal has the same stress state as the macrosCOpIcally applied one. This theory failed to predict the homogeneous deformation. Thus Taylor tried a different theory which avoids this discrepancy by assuming that the strain is the same for all grains. The rolling texture theories assume that the orientations which satisfy both the requirements of a tensile stress parallel to the rolling direction and compressive stress parallel to the sheet normal will constitute the rolling texture. The brass component of the brass type is obtained by the application of Sachs' model to the ( I I I M I0> slip deformation. However, the Taylor theory is more adequate than Sachs's theory in predicting the constrained deformation of the polycrystalline material ,( 4). The calculated texture on the basis of the Taylor theory corresponds well to the experimental texture except the obvious deviation in the region of the rolling direction. Thus Honeff and Mecking (' 5) modified the Taylor theory by introduing the concept of partly constrained deformation of the crystallites. Figure 4(a) shows the shape of an initial cube after about 75% thickness reduction if Taylor's restriction on material flow have been obeyed. Figure 4( b) to 4(d) display schematically respective shapes II one of the three shear components have been freely chosen, Some results of partly (E,o,-E , 0 .0.0I (E,o,-E .0} ,ol IIX K \\ ‘ \ \ \x k} ‘7 y (aI (bl IE.0:€,0c.fl IE.O:€.LOpI _ r\- "' ————— \ \ \ (cl ((1) Figure 4: Shear misfit produced by the three different shear components {at Taylor case.(b)misfit in Gymtclmisfit in remand Id) misfit IE .0. ‘E .°.t .0) (at SO*- SO 0\ P _ "- 1 1 1 0 30 L5 60 90 c, I'I I E.°.-E .°.t. it I (GI 30} O IO (5.0.4.0.0.” lot L l 1 0 I )0 LS 60 90 *PII’I (E .o..E,f,f,il (cl JO LS 60 90 RH IE,0, {,t .o.o) (cl 30’ 1k 1 1 1 0 )0 LS 60 90 fil'l Figure 8; Orientation distribution along the skeleton line as calculated for {I I I} slip according to the theory of relaxed constraints if (a) 6x2 (0) exy (c) eyz (0) 6X2 and 6W (e) all shear strains are assumed to be unconstrained. l I Q ———’ I) O ‘9 C1 ACID...‘ / i5» I.2+ co . 0,I'O!. 08 * 0.4 t . tgc1=€CR <1 A - - A 20 40 60 BO red.I'I-I (a) (bi ‘ (C) Figure 6: (a) ( I I I ) pole figures of act-brass single crystal after unconstrained rolling (or) and after rolling with constraints on 6y? (G), which leads to twinning on the( I I I) plane perpendicular to ID (_ b) Schematic of the shape change of the initially rectangular rolling plane of the crystal. (0) too as a function of the thickness reduction for the cases of unconstrained (or ,I and constrained ([3) deformation cousfvained deformation are shown in Figure 5. The experimentally observed distribution of orientations near {I I2} and { I 23} <634> in figure 4(d) can be explained by the theory of the relaxed constraints for flat grains where the shear misfit in exy and 5x2 is considered to be unimportantThe brass component is due to the uncostraints of Eyz rather than unconstvaiuts of Exy and 6X2. However eyz is not characteristic of the flat grains since there the costraints on eyz are very strong. Thus the development of brass texture has to be explained In a different way, which is possible by taking into account the effect of the anisotropy of the environment of the grains,( 4 ). This aspect is to be considered in textured materials and attains particular Importance in the context of twinning, since twinning leads to fixed orientation relationship between neighboring crystal I I tes. How twinning influences the constraints is shown well in the brass single crystal experiments( 6). After rolling brass single crystal with {I I0} orientation, this remains stable. Thus a shear component eyz which converts the rectangular rolling plane into a parallelogram Is developed. If the same crystal is rolled with constraints on CV2 twinning occurs on ( I I I) plane perpendicular to TD. Thus the single crystal is split into alternating lamellae of twins and matrix, which have the two crystallographically equivalent orientations ( I I0) I- I I2] and (ITO) III2]. These components produce shear strains C‘yz that are opposite in sign and thus cancel each other on the macroscopic scale, so that the internal reaction stresses are drastically reduced. Therefore the crystallites of the two complementary { l IO} < I I 2> orientations slip like unconstrained single crystal. 2.} Annealing Texturfi of FCC Metal}; and Al Igys II a deformed material with a deformation texture is annealed, a recrystallization texture occures in it, which can be either identical to or differerent from the deformation texture. Figure? shows typical texture after rolling and subsequent primary recrystallization in fee. metals. The rolling texture of copper produces the cube texture (a and b) , the brass rolling texture forms the brass recrystallization texture which has {326}<83$> as the main component (8 and f). An the intermediate rolling texture transforms into an intermediate recrystallization texture, to and d). Since a recrystallization texture Is determined by the structure formed during deformation, nucleation from the deformed state Is of primary Interest in recrystallization textures. Many possible nucleation mechanism have been suggested. The most significant nucleation mechanisms (7) are summarized in the following. —‘ . Nucleation at preexisting grain boundaries by strain induced grain boundary motion on moderately deformed materials. I‘x) . Preferred nucleation in regions of strong orientation gradients in heavily deformed materials. . Nucleation by subgrain growth in a homogeneous deformation structure. (.4 However even orientations of high nucleation rate may not exist in the recrystallization texture in practice. Thus the theory of oriented growth was proposed by Beck( 8). According to this theory nuclei with diverse orientations exist In the early stage of primary recrystallization, but then only the nuclei whose orientation relative to the textured deformed matrix provides to the highest mobility of their boundaries will succeed during. In fcc metals grain boundaries with an orientation related to the marix by rotations 400< I I I> have been found as high growth rate boundaries (9). While the orientation of recrystallization nuclei repeats the orientation of the deformed maxtrix the growth rate is the result of the competing Deformation Recrystallization Figure 7 ; ( I I I) pole figures of rolling textures of Cu-Zn alloys before and after recrystallization. (a).(c).and (e) subsequent to rolling with 95% thickness reduction of (a)Cu and(C)Cu-S%Zn at room temperature and (e) (Tu-8% Zn at 770K. (b).(d), and (I) show the corresponding textures after primary recrystallization. effect of the driving and retarding forces , which is determined by the interaction of numerous factors. One or another of these factors decide which of the two processes, either nucleation or grain growth Is predominant. Thus the development of recrystallization textures can be regarded as a conbination of these two theories. 2.4 Theories of the Develooment of Recrystallization Texture. An fcc metal with a low stacking fault energy, if rolled at a low enengy temperature, develops a texture with a strong { I IO}<1 12> component and a somewhat weaker component in {I IO} as in Figure 7. The corresponding texture afterprimary recrystallization again shows maxima of intensity in two positions, namely, rather high intensity In {326}<83S> and slightly less in {013}<100>, as seen in Fig7f. In Figure 8 the precise positions of the poles of the two complementary {I IO} (I and 11) components are shown( IO). I and II are twin related and thus have the peculiar property that from the eight orientations obtained by 400 rotations around the <1 I I > poles of one com ponent, each orientation happens to become a neighbor of one of the eight orientations produced by the 400~ rotations of the other component. Because of the orthorhombic symmetry of the rolling process, the eight possible orientation pairs consist of only three crystallographical Iy different sets One of each set of orientation pairs is given in Fig.80—d. It is a striking fact that the recrystallization components {326}<83‘5> (b). {OI 3}< 100>(c), and {21 I }
    (d) represent fast~—- growing orientations with respect to both {I IO} components of the rolling texture.{2l I}(d) has never been observed In recrystallization textures while {326}<835>( b) {O I 3}< I 00> are observed frequenty. Thus there should be some other selection principles. It seems to be related to the nucleation mechanisms. However there are some observations which do not fit Into the concept of the compromise orientations based on 40' rations. For the Cu—p alloys( 10) different orientation (a) d)(oll)[21ll a (326)[83§] Hfl dxtniiilziil rotated Tl+ I'— I A (326)18351 (c) As (oii)I21il rotated 8+, P+ §.Iol3)[lool (d) as (oiiilziij rotated A+ A (Ziiiloiij Figure 8: commonent T commonent IT 0‘ (oiiilziii 39Q rotations of both components of the. t 01 I )[21 TI orientation relationship between deformation texture and recrystallization texture was found not 40' rotations but 38.9’ rotations shows the heighest growth rate. Upon these rotations four comprimise orientations are found with respect to the (01 I ) <21 I> orientation as illustrated in Figure 9. The two compromise orientations, ( I 13) <332> and (01 I ) < I 00> are observed in practice. Base on these findings it can be concluded that selected growth is the dominant mechanidsm for recrystallization texture development in low stacking fault enery materials. CHAPTER 3 EXPERIMENTAL PROCEDURE AND TECHNIQUES 3. 1 Pole Figure System The orientation distribution of crystallites in polycrystalline materials, to. textures, have been investigated mainly by X—ray texture goniometers. In the following how the goniometer scan a whole pole figure projection will be discussed. 3. I . I Principles of X—ray Texture Goniometers The crystallographic orientation g of an individual crystallite in a polycrystalline sample is defined by the orientation of Its crystal coordinate system KC with respect to the sample coordinate system Ks- The orientation g of KC with respect to KS can be described by the angles a B of a direction Iuvw] and the rotation angle y [uvwl If the direction [uvw] Is the normal to the reflecting lattice plane (hkl) then the reflected intensity is Independent of a rotation of the crystal through angle y. Thus polycrystal diffraction yield the orientation distribution of the crystal direction [uvw] as a function of or and B. This is called as (hkl) pole i’igure( I I ). In orwr to measure the pole figure it is necessary to rotate the shample through three angles is provided This enables one to bring a sample fixed coordinate system KS Into any position with respect to a laboratory system KL. In the start position K3 is paralled to the KL Then the sample is rotalted successively I about Xs through .01 I8 2.about Ys through (P Sabout Xs through to? In the back reflection technique ( 12) a sheet sample is mounted on the sample holder with its normal direction parallel to the axis of the l9? rotation, This leaves the choice of setting the rolling direction parallel to YS or Z s' If we set it as YS the sheet has the orientation. Y5 //RD ,28 //io,xS //ND (I) in the sample holder as shown in Figure 10. Then the sheet Is set at the angles (0 = Oh“. This is shown In Figure 1 I. With <1) and to? In the zero position the diffraction vector d which bisects the angle between incident and reflected beam is parallel to Zs. By the rotation to and 1.02 the diffraction vector is brought Into the position (a,B) as shown In Figure 12. Where a and B are the pole figure angle defined with respect to Its sheet coordinate system RD, TD, NO as shown in Figure I 1. Thus this motion Is characterized by 01 =O=const (2) and the pole figure angles are related to d) and 192 (.4 V a=90~¢ e=90+o2 ( where (it and (.02 are taken positive in the sense of a right handed screw about the YS and X8 directions respectively. 3.1.2 Pole. Figure Protections Most pole figures In the metallurgical literature are projected in the stereographic projection. Because this projection is angle true and measurement of angle is simplfied. 2O Figure 10 : A sheet sample mounted in back-reflection position. Figure I 1 :Starting position of the sample 21 Simultaneous rotations in the a and 0 modes, when the pole figure device is measuring in reflection, cause the normal to the reflecting planes to describe a Spiral in the plane of I stereographic projection, Figure I 3. The Intensity of a pole along the spiral is plotted on the projection. Figure 14 is the Illustration of this principle. The noral CP is represented by its pole p, which is the intersection to p with the reference sphere. The pole p is represented by Its stereographic projection p'. This geometry Is drawn in two dimensions as shown In Figure 18. With this one can derive the radius for a certain position on the pole figure projection. 12' =Rsina/2 (4) lid is too large the irradiated region may become larger. And for out 0 the focussing condition is only fulfilled for the central line of the ample. These conditions reduce the reflected intensity according to at . However, if the reflected intensity is being compared with the corresponding intensity from a random sample,the calculation of the correction factors can avoided ( 13). The calculation of the noralization condition from definition. F’hkl (O‘I3Irandom:1 (5) I. (a8) = l'randomm) phklmfi) (6) Eq( 6) gives the pole density In multiples of the random density. 3.2.3 Installation of Pole Figure System A Norelco wide range goniometer was mounted on a diffractometer base. The collimator was aligned to the "spot focus" window of the X—ray tube (port No.3).ln order to fulfill the geometry of scanning the following conditions were maintained during assemby procedure. I. The distance between the center of the X—ray tube and the center of the sample should be I 70mm. 2 The distance between the top surface of the sample holder and the basic unit RD F Figure 12 ' The diffraction vector d is brought Into the sample direction {ci,G} by the k rotations <1) and to I a raw X-rey beam 6 _——’—-1>-——_ E oniometer axis 1 g detector w \ Figure 13 ' Geometric illistration of axial motion K? \77 C A Figure 14 : The illustration of pole figure projection. C R A Figure 15: The two dimensional Illustration of pole figure projection 24 table top should be 260mm. 3. The distance between the shutter assembly and the collimator should be as short as possible without making contact. 4. An image of the exit opening of the collimator with dimensions of approximately 4X I mm2 rectangular should be visible on the fluorescent disc. An IBM XI computer was adapted to the counter electronics hrough a WB-AIO—B Analog-to digital converter for the automatic determination of pole figures. This analog card was Installed in the connector slots located inside the IBM computer. The recorder output was conneceted to the terminal box. The software of this analog card was set up to select the voltage range as SOmv. This system configuration is shown in Figure 16. In order to check the accuracy of this system, an aluminum single crystal and lithium fluoride single crystal was used as the test material. The orientation of the single cyrystals were determined by Laue patternslhe results are shown in Fig Usually It is not possible to indicate the rolling direction in the pole figure exactly. Thus the rolling direction on the measured pole figure is not in a correct position. It is then more accurate to determine it by symmetry considerations from the pole figure measurements themselves. This is achieved by rotating the pole figure through an appropriate angle. Then the correctly adjusted symmetric pole figure is obtained. The calculation of the correction factors ( Ie geometrical factor, defocusihg factor, and absortion factor) can be avoided If the reflected intensity is being compared with the coerresponding intensity reflected from a random sample under the same conditions. 3.2.4 Software system This system can be divided in three parts as shown in Figure 17. The first is used for data aquisition. The second is the pole figure plotting program The third Is applied to the second part 25 Geiger detector A-D converter Wide range gonnnneter X-rag generator Figure 16 : Pole figure system configuration. Data processing computer hardchsk SCFEBFI floppg <;> disk 2.] printer 26 POLE it 81111: 811’,,..—-—--—--—«..__“_ AAAAAAAAAAAAAA f/.— x\\ 81-38-1988 88:59:23 / \ FILE IIIIIIE : LIF.DAI / \ Hey I IN 38 / \ HII L - III 15 ’I .\_ SCALE 5 1 / " " \ PITCH I 2.5 I \ nor. STEP: 2.5 j z, TD 4» DEN 1011488 I, I till I " 2 91885 \ - '- / 3 14.497 \ ,4 4 19.329 \ 5 24.182 \ 6 28.994 \ . 3 33.826 -\ J/ 1:011: acute off-“Huck AAAAAAAAAA AA x”, x‘x .f’ \ 81-38-1988 81:84:42 / , \'\ FILE IIIIIIE : 4L811.8 / \ X-rag : RU 39 / \ H il (TCE(R-Ad)l/2 Broadening was avoided by a ratio of specimen broadness to thickness b/d > 3. This led to a homogeneous stress state which nearly fulfills the conditions of an ideal plane strain compression. in order to avoid orientation gradients, the specimens were thinned from both faces by mechanical polishing to approximately 0.25mm thick Tablet. The Relation between Axial Motion Data Aquisition Large Small Pitch Number Data Degree Degree per Rotation of Data Aquisition (o/mm) (o/mm) (timer) Scale level Scale level Rotation Step right 5 435/8 1 296 5.555 5 i left 5 l2°ll6 4255/16 2592 2.777 2.5 right 2.5 435/8 2592 5.555 5 2 6°ll6 left 2.5 435/ i 6 5 i 64 2.777 2.5 Table 2. Setting of 26 pole . 111 200 220 material aA cu 3.6146 43.39 50.39 74.26 Ag 4.0779 36.16 44.36 64.56 Cu Tube LiF 4.027 36.66 44.97 65.46 A- 1.54A A1 4.0497 36.46 44.70 65.07 cu 5: Ag 3.624 43.19 50.29 73.66 Cu 2.53 Ag 3.624 43.29 50.42 74.09 Cu 19.59 22.65 32.25 Ag 17.34 20.05 26.51 l‘io Tube LiF i6.56 20.31 26.66 A- 0.71A A1 17.47 22.20 .2672 cu 5: Ag 19.54 22.60 32.17 Cu 2.53 Ag 19.56 22.65 32.24 -.t_.._-_. _ 3.2.2 Heat Treatment of the samples For the rolling textures two types of heat treatment were carried out. These heat treatment schedules are summarized in Figure l 8. The first was used to study the recrystallization behavior of a supersaturated 01 solid solution. It. was annealed at 9000C for 7 hours, followed by water quenching. The second was designed to investigate the rolling and annealing texture development of the two phase material(0t solid solution + 8 solid solution) and accomplished by annealing at 6000C for three hours and then cooled by water quenching. l n order to determine the recrystallization temperature isochronal tests were carried out on both solid solution and two phase material, cold rolled to 95% reduction. The results are plotted as ’isochronal curve‘ in Figure l 9. The major drop in hardness is due to the recrystallization, which occurs between 525 and 575°C in the solid solution sample while a similar drop occurs between 575 and 625°C for the two phase material. The copper-silver phase diagram indicates that the copper alloy containing 5% silver will be in a solid solution between 7800 C and 9800C. Below 7800C the solubilit of silver in copper is less than 5%. Thus ,if the alloy is maintained for three hours back up to 6500C after quenching from homogenizing temperature, 8 solid solution to precipitate. HV 70* i 60'“ 50“ D alpha solid solutuon 40“ 0 two phase a 8 o 9'- . l l i l l 300 400 500 600 700 Figure 19 : Hardness variation during annealing of rolled specimens. T°K CHAPTER 4 RESULTS AND DISCUSSION 4.1 Rollianexture 4. t . 1 Experimental Results Textures were obtained from both ( 1 1 1 ) and (200) reflections by using the Schulz reflection method. Complete pole figures were then obtained by normalizing all data with respect to the random powder specimen. The Cu—Ag alloy( solid solution) rolled to 95% reduction exibits a brass type texture which is superimposed by the brass- and goss- position. These two texture components are presented clearly by the {1 l 1} and {200} pole figures in Figure. Also the Cu-Ag alloy( two phase) rolled to 95% reduction shows a same texture composed of the brass- and pass - orientation like Cu—Ag solid solution alloy. There was no evidence to distinguish the rolling texture of the solid solution alloy from that of two phase alloy. 4.12 Discussion it is common to distinguish between two types of rolling textures at high rolling reduction. One is the copper—( pure metal) type texture at high stacking fault energy and the other is the brass-(alloy) type texture at low stacking fault energy. According to the present result it seems to be obvious that 5% alloy content can decrease the stacking fault energy of Cu—Ag alloy low enough. Thus the transition of the rolling texture observed here for the Cu—Ag al toy is similar to that obversed in the brass and Cu-P alloy( 10). Only the amount of alloy content to cause the transition was different in such a way that 5% Ag corresponds to 14% and 1% P. It shows once again that only one parameter, 1e SFE, is supposed to cause this rolling texture transition. Thus the mechanism of this texture formation can be explained as same as that of brass and 34 Cu—P alloy. In low SFE alloys slip is preferred on planes parallel to the twin boundaries of the fine twin lamella, which leads to an abnormal rotation into the {323M 13> and the {t 1 1}<1 10> positions. The formation of shear bands through these rotated twin regions changes their orentations again to near the goss— and brass- position forming the final brass type rolling texture,( 16). 4.2 Recrystallization Texture 4.2.1 Experimental Results The recrystallization textures of the Cu-Ag solid solution alloy after rolling and annealing at 600 C composes of three main components, the 9033- cube-and {258}{ 121 } —0rientation (about 37°< i 00> orientation relationship to the brass- component). 1f annealed at 550 C, this alloy shows a different texture which is composed of cube- and {258}<121>- component. Obviously some influence is exerted by the annealing temperature, since the texture annealed at 600 C reveals a goss—component in addition to two components present at 550 C. These pole figures are shown in Figure. For the Cu—Ag two phase alloy the recrystallization texture is composed of the goss orientation and {258}<121 > (near brass) position occurs. This is shown in Fig. . 4.2.2 Discussmp 1n the present work, different preannealings influenced the temperature of recrystallization and the textures practically. After primary recrystallization one find relatively different textures for Cu-Ag solid solution alloy and for Cu—Ag two phase alloy. In first case the resulting textures are varying according to the annealing temperature. While the brass component of rollinng disappears the goss component still shows the strong intensity. Thus retained goss component can be explained by the nucleation based on the subgrain‘growth. And the component {258}<121> which has an .37 < 100> orientation relationship to the brass component as in case of Cu-P alloy( 16). And the 36 component {258}<121> seems to be due to the preferred high growth rate. However the origin of the cube component is unknown. It can be pointed out that there should be some interaction between recrystallization and the precipitations from the different annealing textures according to different temperaturesThus the resultant recrystallization texture were influenced to some extent by the temperature and time of annealing. At present, however it is impossible to formulate the conditions to produce this difference. In second case both the goss position and {01 1}<733> position (near the brass component) are strong similar to the rollimg texture. These have a certain similarity to the rolling texture besides the brass component of rolling is rotated about 10 around its <1 10>. One can assume that the small amount of excess 8 sol id solution along the grain boundaries cause the retention and the slight rotation of the brass component. The goss component is again seems to be nucleated by subgrain growth. 1011: 1191191: Ripe-T4. AAAAAAAAAAAAAA {/1}, '. .. .1 ; '1 '- .. .\ 91-39-1991 99: 15 : 59 /. 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STEP i 2.5 TD DEN X*ROUDOH 518 92229 9.922 flmmpwmr—a-(D 24 26 28 29 31 Fi'ur"‘7 " 3‘ ” ‘ ‘" ' ' g e 4191 ll l l,( 2-00) pole iigures 01 recrvstallizatiun textures of Cu-S%Ag two phase al lav after ml 1 mg and ani‘iealing at 1513100122 CHAPTER 5 SUMMARY AND CONCLUSIONS in the present paper textures were obtained from both ( l l i)and (200) reflections by using the Schulz reflection. Complete pole figures were then obtained by normalizing all data with respect to the random powder specimen. The transition of the rolling texture observed here for both the Cu-Ag solid solution alloy and the Cu-Ag two phase alloy is similar to that observed in the brass and Cu-p alloy. Only the amount of alloy content to cause the transition was different. It shows again that only one parameter ,i.e. SFE, is supposed to cause this rolling texture transition. After primary recrystallization one find relatively different textures for the Cu-Ag solid solution alloy and for the Cu-Ag two phase alloy. in first case the resulting textures are not brass recrystallization textures and are varying according to the annealing temperatures. in second case the resultant textures have a certain similarity to the rollingtextures besides the brass component of rolling is rotated about 100 around its <1 10>. The recrystallization textures depend first on therolling textures which is determined by the SFE. Secondly it depends on precipitates along the grain boundary. These complicated dependencies are the reason for the variety of recrystallization textures as com pared to rolling textures. BIBLIOGRAPHY l. G.WASSER11ANN,1J.GREWEN, Texturen metallischer Werkstoffe, Springer—verlag, Berlin/Gottingen/Heidelberg( 1962). 2. R.ALAM ,H.D.MENGELBERG,and K. LUCKE, [Metallkde S8 ( 1967) 867. 3. GWASSERMANN, Z.Metallkde S4( 1963) 61. 4. HMECKING. int. Conf. on Textures, Vol. l,Tokyo( 1981) 87. 5. 1111011999, HMECKING, INT. Conf. on Textures. Vol. 1 ,Aachen ( 197a) 2959.,” 6. HMECKTNG. Int. Confon Textures, Vol. 1,Aachen ( 1978) 2S. 7. G.GOTTSTElN,lnt. Conf. on Textures, Vol. 1,Aachen( 1978) 96. 8. P.A.BECK,Acta Met, 1(1953)230. 9. B.LlEBMANN, K.LUCKE,and GMASINO, [Metallkde 47(1956)S7. 10. U.SCHMIDT,K.LUCKE. and J.POSPIECH,Int. Conf. on Textures, Cambridge( 1975) 154. l1.H.1}.BUNGE,K.H.PUCH,Z.l“letallkde 75(1984) 124. 12. L.G.SCHULZ,J.Appl.Phys. 20( 1949) 1030. 13. H.J.BUNGE Texture Analysis in Materials Science, Butterworty, London ( 1982) 92. 14.E.A.OWEN,1J.ROOERS.Jlnstflet.S7(193S)2S7. 15.K.LUCKE, int. Conf. on Texture, Vol. 1,Tokyo( 1981) H 16.J.H1RSCH, K.V1RNICH, and K.LUCKE. Int Conf. on Textures, vol. 1 , Tokyo( 1981) 37S. 44 11111111 7 3 6 2 2 6 o 3 0 3 9 2 1 3 1l111111111111111111