21 4 2011 4 Vol.21 No.4 The Chinese Journal of Nonferrous Metals Apr. 2011 1004-0609(2011)04-0708-06 Al-4.74Cu-0.50Mg-0.30Ag X 1 1 1 1 2 1 3 (1., 100088 2. 100088 3. 201204) X (SAXS) (TEM) Al-4.74Cu-0.50Mg-0.30Ag Ω θ TG 146.2 A Small angle X-ray scattering study of Al-4.74Cu-0.50Mg-0.30Ag alloys during aging process ZHANG Jian-bo 1, ZHANG Yong-an 1, ZHU Bao-hong 1, WANG Feng 1, ZHENG Yi 2, XIONG Bai-qing 1, WANG Yu-zhu 3 (1. State Key Laboratory for Fabrication and Processing of Nonferrous Metals, General Research Institute for Nonferrous Metals, Beijing 100088, China; 2. Department of Powder Metallurgy, Central Iron and Steel Research Institute, Beijing 100081, China; 3. Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204, China) Abstract: The precipitation behavior of Al-4.74Cu-0.50Mg-0.30Ag alloys during single aging process was studied by the synchrotron-radiation small angle X-ray scattering (SAXS), transmission electron microscopy analysis (TEM) and mechanical property test. The results show that the Ω phase and little θ phases precipitate during single aging process, and with prolonging the aging time, the radial size of the precipitates increases notably, whereas the width of the precipitates increases little, therefore, the shape of the precipitates gradually changes into thin plates. The size of the precipitation increases at the beginning of aging process and goes to a stable value at last. The volume fraction of the precipitation increases at the beginning and then decreases, at last increases in a smaller rate. Key words: aluminum alloys; small angle X-ray scattering; precipitation; volume fraction Al-Cu-Mg-Ag, [1] Cu/Mg Al-Cu-Mg GP ( {100} ) θ θ θ Ag Al-Cu-Mg (150 ) Ag Al-Cu-Mg-Ag GPB ( {111} (50904010) 2010-04-16 2010-07-29 010-82241165 E-mail: zhang4318@163.com
21 4 Al-4.74Cu-0.50Mg-0.30Ag X 709 ) Ω θ θ Ω [1 2] (TEM) (HREM) Ω [2 6] HONO [7] TEM X RINGER [8] TEM Ω θ Ω 200 SONG [9] TEM / LIU [10] TEM TEM X X Al-Li Al-Zn-Mg-Cu Al-Li-Mg-Cu Al-Mg-Si [10 14] Al-Cu-Mg-Ag X SAXS Al-4.74Cu-0.50Mg-0.30Ag ( ) Al-Cu-Mg-Ag X 30% + 70% ( ) 16~18 V 70~90 ma 30~ 20 JEM 2000FX TEM 1.3 X X (Small angle X-ray scattering, SAXS) X ρ ρ 0 (ρ ρ 0 ) 2 X X X 25 mm 25 mm 0.13 mm 5~20 kev 10 kev 6 10 4 1 10 11 S 1 0.5 mm 0.5 mm λ 0.124 nm 4 10 4 rad(0.023º) 2 2.1 1 Al-Cu-Mg-Ag 160 180 1 1.1 ( ) Cu 4.74% Mg 0.50% Ag 0.30% Al 12.3 520 2 h 160 170 180 200 1.2 GB/T16865 97 TEM 1 Al-Cu-Mg-Ag 160 180 Fig.1 Yield strength aging time curves of Al-Cu-Mg-Ag alloy at 160 and 180 during single aging
710 2011 4 160 10 h 180 4 h 450 MPa 180 160 2.2 160 180 Al-Cu-Mg-Ag 2 110 α 2(b) (d) (f)tem (1/3) {022} (2/3) {022} 110 α Ω (1/2){022} 001 θ 2(a) (c) (e) TEM Ω θ (2~10 h) (10~28 h) 2 Al-Cu-Mg-Ag Fig.2 TEM bright field images ((a), (c), (e)) and corresponding selected area electron diffraction patterns ((b), (d), (f)) of Al-Cu-Mg-Ag alloy during single aging process: (a) T6 temper; (a), (b) 160, 2 h; (c), (d) 160, 10 h; (e), (f) 160, 28 h
21 4 Al-4.74Cu-0.50Mg-0.30Ag X 711 2.3 X 2.3.1 X 3 [15] FIT2D 0~360 SAXS 4 (160, 20 min) (160, 8 h) Guinier I(h) h h=4πsinθ/λ 2θ λ 2.3.2 Guinier [16] e 2 2 2 G Ih ( ) = INn exp( Rh /3) (1) I(h) I e n N X R G 3 (a) Guinier ln I(h) h 2 ( 4(b)), Guinier α, R = α (2) G 3 R 3 X Fig.3 SAXS results of alloys after different heat-treatments: (a) 180, 20 min; (b) 180, 1 h; (c) 180, 4 h; (d) 180, 40 h
712 2011 4 4 Guinier Fig.4 Scattering and Guinier curves under different aging conditions: (a) I(h) vs h; (b) ln I(h) vs h 2 5 Fig.5 Relationship between gyration radius and aging temperature and time R R G = (3) 2 4(b) 5 5 Al-Cu-Mg-Ag Ω [17] 2.3.3 0 2 2 2π 2 2 2 2 p m ϕ ϕ Vat Qh = I( h) h d h= ( Z) ( c c ) (1 ) (4) I(h) V at Al ( 16.6 Å 3 ) Z Al c p c m ϕ ( ), 6 ϕ 0.5, ϕ( 1 ϕ), ϕ [11] 0.5 6
21 4 Al-4.74Cu-0.50Mg-0.30Ag X 713 ratios[j]. Acta Materialia, 1996, 44: 1883 1898. [6] RINGER S P, SAKURAI T, POLMEAR I J. Origins of hardening in aged Al-Cu-Mg-(Ag) alloys[j]. Acta Materialia, 1997, 45: 3731 3744. [7] HONO K, SANO N, BABU S S, OKANO R, SAKURAI T. Atom probe study of the precipitation process in an Al-Cu-Mg-Ag alloys[j]. Acta Metallurgica et Materialia, 1993, 41: 829 838. [8] RINGER S P, YEUNG W, MUDDLE B C, POLMEAR I J. Precipitate stability in Al-Cu-Mg-Ag alloys aged at high-temperature[j]. Acta Metallurgica et Materialia, 1994, 42: 1715 1725. [9] SONG M. Modeling the hardness and yield strength evolutions 6 160 180 SAXS Fig.6 Relationship between integrated intensity and aging time at 160 and 180 3 1) Al-Cu-Mg-Ag 2) 160~200 50 h 3) ( ) REFERENCES [1] POLMEAR I J, PONS G, BARBAUX Y, OCTOR H, SANCHEZ C, MORTON A J, BORBIDGE W E, ROGERS S. After Concorde: evaluation of creep resistant Al-Cu-Mg-Ag alloys[j]. Materials Science and Technology, 1999, 15: 861 868. [2] GARG A, HOWE J M. Nucleation and growth of Ω phase in Al-4.0Cu-0.5Mg-0.5Ag alloy An in situ hot-stage TEM study[j]. Acta Met Mater, 1991, 39: 1925 1937. [3] HOWE J M. Analytical transmission electron microscopy analysis of Ag and Mg segregation to {111} thetas precipitate plates in an Al-Cu-Mg-Ag alloy[j]. Philosophical Magazine Letters, 1994, 70: 111 120. [4] HONO K, SAKURAI T, POLMEAR I J. Pre-precipitate clustering in an Al-Cu-Mg-Ag alloy[j]. Scripta Metallurgica et Materialia, 1994, 30: 695 700. [5] RINGER S P, HONO K, POLMEAR I, SAKURAI T. Nucleation of precipitates in aged Al-Cu-Mg-(Ag) alloys with high Cu:Mg of aluminum alloy with rod/needle-shaped precipitates[j]. Materials Science and Engineering A, 2007, 443: 172 177. [10] LIU G, ZHANG G J, DING X D, SUN J, CHEN C H. Modeling the strengthening response to aging process of heat-treatable aluminum alloys containing plate/disc- or rod/needle-shaped precipitates[j]. Materials Science and Engineering A, 2003, 344: 113 124. [11] DU Z W, SUN Z M, SHAO B L, ZHOU T T, CHEN C Q. Quantitative evaluation of precipitates in an Al-Zn-Mg-Cu alloy after isothermal aging[j]. Materials Characterization, 2006, 56: 121 128. [12],,. Al-Zn-Mg-Cu [J]., 1997, 33: 479 484. MENG Zhao-fu, ZHENG Yong, LONG Hou-wen. Hardness changes of Al-Zn-Mg alloy during retrogression and reaging[j]. Acta Metallurgica Sinica, 1997, 33: 479 484. [13],,,. X Al-Li δ [J]., 1999, 7: 71 73. CHAI Zhi-gang, YU Yan, MENG Fan-ling, MENG Zhao-fu. Determination of activation energy for growth of δ in Al-Li alloy by SAXS[J]. Material Science & Technology, 1999, 7: 71 73. [14] TSAO C S, JENG U S, CHEN C Y, KUO TY. Small-angle X-ray scattering study of nanostructure evolution of β precipitates in Al-Mg-Si alloy[j]. Scripta Materialia, 2005, 53: 1241 1245. [15]. [M]. :, 2008: 33 34. ZHU Yu-ping. Small angle X-ray scattering[m]. Beijing: Chemical Industry Press, 2008: 33 34. [16] GUINIER A. Small-angle scattering of X-rays[M]. New York: John Wiley & Sons, 1955: 28 29. [17] HUTCHINSON C R, FAN X, PENNYCOOK S J, SHIFLET G J. On the origin of the high coarsening resistance of Ω plates in Al-Cu-Mg-Ag alloys[j]. Acta Materialia, 2001, 49: 2827 2841. ( )