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1、46720107769774ACTA METALLURGICA SINICA Jul. 2010pp.769774 Cu(,255049(,255049(EBSDCu(GBCD.,(12µm75.7%3n (n =1,2,3,3n (n =1,2, 3 ,200µm,GBCD;,. EBSD(twinltering(FPM,(triplejunctions3,3GBCD ,GBCD.Cu,TG111A0412 1961(201007 0769 06EFFECT OF GRAIN SIZE ON THE GRAIN BOUNDARYCHARACTER DISTRIBUTION
2、S OF COLD ROLLED AND ANNEALED PURE COPPERCAI Zhengxu, WANG Weiguo, FANG XiaoyingSchool of Mechanical Engineering, Shandong University of Technology, Zibo 255049GUO HongCenter of Testing and Analysis, Shandong University of Technology, Zibo 255049Correspondent:WANG Weiguo, professor, Tel:(05332786835
3、, E-mail:wang.wei.guo Supported by Nature Science Foundation of China (Nos.50771060and 50974147 Manuscript received 20100206, in revised form 20100420ABSTRACT Pure copper (99.97%samples with varied grain sizes were cold rolled and annealed at rst and then their grain boundary character distributions
4、 (GBCDswere characterized by electron back scatter diraction (EBSDtechniques. The results showed that the sample with ner initial grain size (12m appeared to be largely populated by the so-called special boundaries such as 3n (n =1,2, 3 after cold rolling and annealing, the fraction of 3n boundaries
5、 reached 75.7%and the averaged size of clusters of grains with 3n (n =1,2, 3 orientation relationships (3n CG were as large as 200m in this sample. However, with initial grain size increasing, the fraction of special grain boundaries as well as the size of 3n CG in the samples were decreasing dramat
6、ically. In situ EBSD observation, twin-ltering and ve parameter method (FPManalyses indicated that triplejunctions are the preferred sites for the nucleation of incoherent 3boundaries which play a important role in enhancing the fraction of special boundaries. It accounts for primarily the desired G
7、BCD results as obtained in the sample with ner initial grain size.KEY WORDS pure copper, grain boundary character distribution (GBCD,grain size, triplejunctions(EBSD*5077106050974147:20100206,:20100420:, 1985,(GBE(GBCD1 3.GBCD4, (anneal-ing twinGBE5, 6., ,7, 8910, 1177046GBCD , 70%,3n (n =1,2, 3200m
8、., fcc GBCD , 10, 1130% 270GBCD ;( , 30486% 900(1050 GBCD ., (strain induced boundary migration, SIBM , GBCD 12, 13. GBCD, GBE ,GBCD .GBCD.14,GBCD ,GBCD . 15( , GBCD. , Wang 16GBCD , , , GBCD ; , , GBCD . GBE 30%,EBSD ,(TEM14, GBCD.Cu fcc ,. Cu, ,Cu GBCD . 17, 10%Cu GBCD . , Cu GBCD ,.,Cu GBCD . Cu
9、, EBSD , GBCD,GBCD.199.97%( Cu . , 10504h , 90% . 3, 900 0.5, 510min ,12, 2035m 3, 1. 3A, B C , 3 n 1A, B C(OIMFig.1Orientation imaging microscopy (OIMof samples A (a,B (band C (cshowing the dierence of av-eraged grain sizes (A,B and C are cold rolled and annealed pure Cu with dierent grain sizes7:C
10、u 771(n =1,2, 3 41.8%,41.9%43.7%. , 310% , 6505min., . HKL EBSD FEI Sirion200(SEM, Kikuchi , (OIM,Brandon 18 ( 15 1/2 ,. , 3500m ×400m , EBSD 2m.GBCD ,(0.4m EBSD .3GBCD , (twinltering 19(ve parameter method, FPM 20, 243.(1113 3, , . FPM , 3(001,MRD(multiplesof random distribution .223A, B CEBSD
11、 OIM , 1GBCD . , A, B C GBCD (3n , GBCD .1, A, B C (10% (650 (5min, 3n , 12, 2035m. 2 1, 3n 75.7%. , , , A 75.7%B 70.1%,C 56.1%.GBCD ;, ,. 2A, B C 10%, 6505min EBSDFig.2Grain boundary reconstructions from EBSD map-ping for samples A (a,B (band C (cafter cold rolled by 10%and annealed at 650for 5min
12、(thin grey lines denote special boundaries including 3,9,27and other low CSLboundaries, black lines denote random high angle boundaries (HABsor ran-dom boundaries, , (SIBM12, .4A EBSD . 4a , 4b ( 10%6502min . ,77246 3A, BC10%, 6505min(OIMFig.3Orientation imaging microscopy (OIMfrom EBSD mapping for
13、samples A (a,B (band C (ccold rolledby 10%and annealed at 650for 5min1A, B C 10%, 6505min EBSDTable 1GBCD results obtained by EBSD for the samples A, B and C cold rolled by 10%and annealed at650for 5min(Lengthfraction, %Sample 139+27Total low CSL 410%6502min A EBSDFig.4Insitu observations of an area
14、 located on the crosssection of negrained sample A(ainitial state(bcold rolled by 10%and annealed at 650for 2min(csinglesection trace analysis for determining the character (coherentor incoherent of 3at two triplejunction A in Fig.4b (N1and N2are the normal directions of grain boundary segments betw
15、een grain G 1and G 2(dsinglesection trace analysis for determining the character (coherentor incoherent of 3at two triplejunction B in Fig.4b (N3,N4are the normal directions of grain boundary segments between grain G 3and G 4(4abAA,(4abBB. 21,7:Cu773(111(4cd,(3.,33n .5A10%6502minEBSD,(5. Miura 22Cu
16、3., A,BC,A 5A10%, 6502min EBSDFig.5Grain boundary reconstruction of a cross-section ofnegrained sample A after cold rolled by 10%and annealed at 650for 2min (arrowsindicate the twins3,GBCD.6AEBSD.6a,6b 10%6503min. ,A B, C3(6ac.EBSD ,ABC3.3, BC.AD,27,CE(6b.,AD ,27,3,23.,3GBCD , 3GBCD. ,GBCD,3. A, BC3
17、. 2,A3B,C, .7A, BC 33(001.,33111,111.3111,(111 610%6503min A EBSDFig.6Insitu observations of an area located on the cross-section of negrained sample A(ainitial state(bcold rolled by 10%and annealed at 650for 3min(corientation relationships between grains A and B, A and C 774 2
18、01; Åß ³Ê ¦ Ï A, B 650 ¨Ð 5 min § ¥ · À ³ 3 ¡ 46 C 10% 3 Table 2 Statistical of coherent and incoherent 3 boundaries in the samples A, B and C cold rolled by 10% and annealed at 650 for 5 min (length fraction, %
19、 Samples A B C 3 59.1 55.2 51.8 3c 36.6 33.8 36.3 3ic 22.5 21.4 15.5 *: 3c and 3ic denote the coherent and incoherent 3 boundaries, respectively Ù ²ÊË Cu ¬ ² Ú·°¹ ¹ÄÜ ¶¼ ¬ ¬ ¿. ²Ê¶ ß Cu
20、 Î ¶ À ¯ GBCD ÜÙ Ì , ²Ê Ñß Cu Î ¶². ½ ² Ç ¬ ÉÇ 3 ² 3 ² ß Ù ß ÄÀÎ , GBCD ß , ²Ç²ÊË ßÎ ¶ ¬ , ¯ GBCD
21、220;Ù Ì ßÆÔ. Ü ¥¦ £ 7 Fig.7 Distributions of grain boundary planes of 3 boundaries in sample A (a, B (b and C (c after cold rolled by 10% and annealed at 650 for 5 min (data are plotted in stereographic projection along 001, the 111 misorientation axis is
22、 marked at red zone Ï C µ 10% Ï 650 ¦« 3 ± Ô ¸ (001 ±Ô Þ¡Û A, B Í 5 min Þ ¥ ²Õ ßÔ 3 ² , ²¦¦ 4 Û° 2 Ï ß ÆÇ ß. 3 ² Õ°¹ 111
23、3;°¿Ç ª ¼, °Ø 3 ² ß Ç¼ ¼. ½ ¤Î B C, Î A ß ¿Çª ¼, Ô ¯ 3 ² ß Ç ¼. 1 Watanabe T. Res Mech, 1984; 11: 47 2 Palumbo G, Erb U. MRS Bull, 1999; 11: 27 3 Kumar B R, Das S K,
24、 Mahato B, Das A, Chowdhury S G. Mater Sci Eng, 2007; A454455: 239 4 Wang W G. Mater Sci Forum, 2007; 539543: 3389 5 Randle V. Acta Mater, 1999; 47: 4187 6 Shimada M, Kokawa H, Wang Z J, Sato, Y S, Karibe I. Acta Mater, 2002; 50: 2331 7 Michiuchi M, Kokawa H, Wang Z J, Sato Y S, Sakai K. Acta Mater,
25、 2006; 54: 5179 8 Fang X Y, Zhang K, Guo H, Wang W G, Zhou B X. Mater Sci Eng, 2008; A487: 7 9 Xia S, Zhou B X, Chen W J, Wang W G. Scr Mater, 2006; 54: 2019 10 Wang W G, Zhou B X, Feng L. Acta Metall Sin, 2006; 42: 715 ( , , . , 2006; 42: 715 11 Wang W G, Guo H. Mater Sci Eng, 2007; A445446: 199 12
26、 Humphreys F J, Hatherly M. Recrystallization and related annealing phenomenon. Oxford: Elsevier Ltd, 2004 13 Fang X Y, Wang W G, Cai Z X, Guo H, Zhou B X. Mater Sci Eng, 2010; A527: 1571 14 Wang W G, Yin F X, Guo H, Li H, Zhou B X. Mater Sci Eng, 2008; A491: 199 15 Zhang X, Wang W G, Guo H, Jiang Y. Acta Metall Sin, 2007; 43: 454 ( , , , . , 2007; 4
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