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- ふみな しどり
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2 Severe Plastic Deformation and Mechanical Properties of Magnesium Alloy Jie XING ABSTRACT Severe plastic deformation (SPD) and the mechanical properties of Magnesium (Mg) alloy AZ31 were studied in multi-directional forging (MDF) under decreasing temperature conditions. MDF was carried out up to a cumulative strain of 5.6 with changing the loading direction during decreasing temperature from pass to pass. MDF can accelerate the uniform development of much finer grain structures in high strain, and the minimal grain size of 0.23µ m can be developed by continuous dynamic recrystallization at 403K. The fine-grained alloy shows higher strength as well as rather high ductility at room temperature and also superplastic elongation in low temperature. The relationship between the grain size and the yield stress or hardness at room temperature can be represented by a Hall-Petch equation. Superplasticity appears even at a low temperature of 393K with a stress exponent of around 5.6 and a total elongation of over 370%. This relative large stress exponent can be connected with grain coarsening or refinement taking place during tensile deformation. A strong deformation texture, i.e. the (0001) basal plane parallel to tensile axis, exits stably during superplasticity. It is concluded that superplsaticity of fine-grained Mg alloy can i
3 be controlled by grain boundary sliding and at the same time grain growth and refinement take place during deformation, while grain rotation hardly takes place. The effect of anisotropy on superplasticity was also studied in MDFed Mg alloy. Tensile test specimens were cut from the MDFed plate parallel (90 specimen), with an inclination angle of 45 (45 specimen) and perpendicular (0 specimen) to the final compression axis. Superplasticity shows the following remarkable anisotropic behaviors. In the 0 specimens, the texture change hardly takes place during superplastic deformation; i.e. no grain rotation occurs. In the 45 and 90 specimens, in contrast, lower flow stresses as well as larger elongations appear accompanying with grain rotation. It is concluded that superplasticity or large elongation of Mg alloys can be controled not only by the grain size, but also the texture of Mg products. ii
4 (Mg) (Mg) (OM) (TEM) 32 I
5 (1) 36 (2) (1) 40 (2) (1) 61 (2) 63 II
6 (1) (2) (1) 85 (2) SEM/EBSD III
7 SEM/EBSD IV
8 1.1 (Mg) 1800 (Al) 1) Mg Al Mg Mg 1950 Al Mg Al Mg 2) 1) Mg 1
9 Mg Mg Mg Mg 1.2 (Mg) Mg (hcp) Fig.1-1 { } { } { } { } (basal slip) (prismatic slip) (pyramidal slip) a c (Fig.1-1 ) 1120 a a+c Mg Mg 2
10 { 1012} { 1012} tension twin c c c 3) Fig.1-2 4,5) MPa 40MPa 5 Mg a Mg 6) 3
11 { 0001 } 1120 { 1010} 1120 { 1011} 1120 { 1122} c a (a) (b) (c) Fig.1-1 Slip systems of Magnesium. (a) basal slip, (b) prismatic slip and (c) pyramidal slip. Fig.1-2 Critical resolved shear stress of basal and non basal slip in Magnesium 4,5). 4
12 1.2.2 Mg 7,8) Mg (Fig.1-2) Mg (1.2.4 ) Mg σ ) ( d ) ( y Hall-Petch (1) (1) 1/ 2 σ y = σ 0 + kd σ k 0 Hall-Petch Fig.1-3 Mg Mg-0.2%Al (0.2% ) 9) k Fig.1-3 Mg Mg-0.2%Al 25 k MPa m 5
13 Fig.1-3 Relationships between yield stress and grain size in pure Mg and Mg-2%Al alloy at various temperatures 9). 6
14 Mg k =280MPa m Al 68MPa m Mg 10) Mg 60µ m µ m 11) Mg 12,13) hcp 14) 22.3µ m AZ31Mg 673K 0.73Tm Tm Mg 673K s -1 σ ε Fig.1-4 Fig.1-4(a) σ ε p 0.12 Fig.1-4(b) 0.3 (Fig.1-4(c)) 7
15 C.A Fig.1-4 Optical microstructures and true stress-true strain ( σ ε) curves of AZ31 alloy deformed to various strains at 673K and at s -1. (a) ε =0, (b) ε =0.1, (c) ε =0.3 and (d) ε = ). 8
16 0.5 (Fig.1-4(d)) Fig Fig.1-5 ε ,16) Fig.1-5(a) ε 0.25 Fig.1-5(b) Fig.1-6 (Fig.1-6(a)) 90 (Fig.1-6(d)), Mg hcp hcp (Fig.1-6), 14) 9
17 C.A Fig.1-5 Surface morphology of AZ31 alloy deformed to (a) ε = 0.1 (OM) and (b) ε = 0.25 (SEM) at 673 K and at s -1 14). N.D (a) (b) (c) (d) Fig.1-6 Inverse pole figures evolved in AZ31 alloy during hot deformation at 673K and at s -1, (a) ε =0%, (b) ε =0.3, (c) ε =0.5, and (d) ε =0.8 14). 10
18 1.3 (Mg) ) ( ) ( ) % 10µ m 0.5Tm(Tm ) (10-4 s -1 ) 10MPa % 18) ( ) 18) σ Kε& m = (2) ε& K σ m ( 0 m 1) m m Mg 11
19 Fig.1-7 AZ91 573K 19) Mg 20) 20) 12
20 Fig.1-7. The variation in (a) flow stress and (b) elongation to failure as a function of strain rate in AZ91 with various grain sizes 19). 13
21 1.3.2 Mg (1) (2) (3)Mg (4) Mg AZ61 10%, 583K 10 6~11µ 1) Mg-8.5Li 473K 85% 623K 10µ 21) ZK60 583K 100:1 3 µ 22) Al ( ) Mg 1 µ 14
22 523K 100:1 0.5µ 23) 4 1 µ (Equal-Channel Angular Pressure; ECAP) 24) (Accumulative Roll Bonding;ARB) 25) (Multi-Directional Forging; MDF) 27) ECAP (Fig.1-8(a)) ARB Fig.1-8(b) 2 MDF 90 (Fig.1-8(c) 15
23 (b) (c) Fig.1-8 Schematic illustration of (a) equal-channel angular p ressure (ECAP), (b) accumulative roll b onding (ARB) and (c) multi-directional forging (MDF). 16
24 26) Al MDF µ m 26-28) 1.4 (Mg) Mg Mg 90 (MDF) 2 Mg 3 Mg 17
25 Mg 4 Mg AZ s K 423K 5 Mg Mg 7 1) ( ) (2000). 2) B.L.Mordike and T.Ebert: Mater. Sci. Eng., A. 302 (2001), 37. 3) 54 (2004), ) 10 (1963), 91. 5) H.Yoshinaga and R.Horiuchi: Mater. Trans., 4 (1963), ) R.Ohyama, J.Koike, T.Kobayashi, M.Suzuki and K.Maruyama: Mater. Sci. Forum., (2003), ) 18
26 64 (2000), ) X.Yang, H.Miura and T.Sakai: Mater.Trans., 46 (20005), ) F.E.Hauser, P.R.Landon, and J.E.Dorn: Trans. AIME, 206 (1956), ) G.Neite, K.Kubota, K.Higashi and F.Hehmann: Mater. Sci. Tech., 18 (1996), ) J.A.Chapman and D.V.Wilson: J. Jnst. Metals, 91 ( ), ) T.Sakai and J.J.Jonas: Acta Metall., 32 (1984), ) T.Sakai: Thermomechanical Processing of Steels (J. J. Jonas Symposium), eds. S.Yue and E. Essadiqi, TMS-CIM (Montreal), (2000), ) 52 (2002), ) H.Higashida, J.Takamura and N.Narita: Mater.Sci.Eng., 81 (1986), ) F.J.Humphreys and M.Hatherly: Recrystallization and Related Annealing Phenomena, Pergamon, (1995). 17) JIS H ) O.D.Sherby and J.Wadsworth: Prog. Mater.Sci., 33 (1989), ) M.Mabuchi, T.Asahina, H.Iwazaki and K.Higashi: Mater. Sci. Tech., 13 (1997), ) T.G.Nieh, J.Wadsworth and O.D.Sherby: Superplasticity in metals and ceramics,(cambridge University Press, 1997). 21) K.Higashi and J.Wadswotrth: Mater. Lett., 10 (1991), ) H.Watanabe, T.Mukai and K.Higashi: Scripta. Mater., 40 (1999),
27 23) H.Watanabe, T.Mukai, M.Mabuch and K.Higashi: Scripta. Mater., 41 (1999), ) R.Z.Valiev, R.K.Islamgaliev and I.V.Alexandrov: Prog. Mater. Sci., 45 (2000), ) N.Tsuji, Y.Ito, Y.Saito and Y.Minamino: Scripta Materialia, 47 (2002) ) A.Belykov, T.Sakai and H.Miura: Mater. Trans., 41 (2000), ) A. Belyakov, K.Tsuzaki, H.Miura and T.Sakai: Acta. Mater., 151 (2003), ) O.Sidikov, T.Sakai, A.Goloborodko, H.Miura and R.Kaibyshev: Philos. Mag., 85 (2005),
28 ) 21
29 2.2 Al Zn Mn Cu Si Fe Mg AZ remain Table 2-1 Chemical compositions of AZ31 magnesium alloy (mass%) mm AZ31 Table mm 21mm 14mm( 2.22:1.49:1) (Fig.2-1(a)) 733K 7.2ks 22.3µ m 6 Mg Fig.g.2-1(b) (a) (b) 40 Fig.2-1 Dimensions of compression sample in mm.(a) small specimens and (b) big specimens. 22
30 60mm 40mm 27mm 55mm AZ31 733K 7.2ks 33.6µ m Fig.2-2 (Constant Strain Rate Apparatus; CSRA) 3) 0.8s PID 1350K 23
31 Fig.2-2 Schematic illustration of the essential components of the compression testes used. 24
32 (DAG 154) ε = H H 0 S S ε& 0 dε 1 dh S ε& = = = (2-1) dt H dt H S 0 ε& = S 0 0 / H 0 H H 0 & ε = ε 0 = & ε exp( ε ) H (2-2) ε& ε& 0 (2-1) S S0 H = ε& H (2-3) H = 0 0 ε& S 0 H S t S = S 0 exp( ε& 0 t) (2-4) 25
33 H 0 H H S (2-3) H 0 0 D/A S V/F CSV ) (1.2.4 ) (Multi-Directional Forging; MDF) MDF 90 ε = 0.8 (Fig.2-3) ε (2.22:1.49:1) 1 26
34 Fig.2-3 Schematic illustration of multi-directional forging (MDF). 1 L L L x 8 ε = 0. Lz x = ln = 0. 8 (1) L x 1 y = z = x = 0.4 (2) 2 L = 1 (1),(2) L = = 1.49 z ε = x x y L y z 27
35 Fig.2-4 3mm 6mm R mm R 1mm Fig.2-4 Dimension of tensile sample in mm s s -1 MDF kgN 6) mms mms ε& = s 1 4 Fig
36 0.3mm PID 20A 2000Ks -1 29
37 Fig.2-5 Schematic illustration of the tensile testing equipment. 30
38 (OM) =7:2:1( ) 19.5V 10s~15s 20ml 3mg 50ml 200ml 2~4s, (TEM) JEM-2010 (Transmission Electron Microscope; TEM) 200KV (6µ m) 0.2mm 0.15mm Tenupol-5 31
39 5.3g 11.6g 500ml 2n 100ml 66~70V (OM) ( PME3) 20~ (TEM) ( ) ( ) ( ) 3 ( ) 100 TEM TSL TOCA(Tools for Orientation and Crystallographic in TEM) 32
40 2.6.5 SHIMADZU HMV N 15s ) 40 (1976), ) 67 (1981), 3) 55 (1991), ) 51 (2001),503. 5) X.Yang, H.Miura and T.Sakai: Mater. Sci. Forum., (2003), ) X.Yang H.Miura and T.Sakai: Mater. Trans., 43 (2002),
41 3 3.1 (Mg) (HCP) 1) 2) Mg (1)Mg AZ31 (2) 90 (3) 3.2 Mg AZ31 Table mm 21mm 14mm( 2.22:1.49:1) (Fig.2-1(a)) 733K 7.2Ks 22.3µ m Pa K 673K ε& = 3 10 s 623K 34
42 3 ε& = 3 10 s 1 90 (Fig.3-1) (TEM) 200KV 600 Temperature, T/K WQ WQ WQ WQ WQ WQ WQ Cumlative strain, Fig.3-1 Schematic illustration of multi-directional forging (MDF) under decreasing temperature con d i t i o n s. 35
43 MDF 3mm 6mm 0.7mm MDF (CA) (TA) CA 10-3 Pa 3) s (1) s -1 ( σ ε) Fig K σ ε 4) 523K 2 473K σ ε
44 True stress, /MPa T=473K T=523K T=573K T=623K AZ31 = s -1 0 T=673K True strain, Fig.3-2 True stress-true strain curves of AZ31 alloy during single pass compression at a strain rate of s -1 and at various temperatures. 37
45 (2) 623K s -1 ( Σ ε) Fig.3-3 Σ ε 493K 473K MPa (Fig.3-2) 473K Mpa 1/3 0.5Tm( 443K Tm ) 403K
46 True stress, /MPa AZ31 = s K 493K 523K 623K 443K (0.5 Tm ) 423K 403K Cumulative strain, Fig.3-3 Typical true stress-true strain curves of Mg alloy AZ31 during MDF at a strain rate of s -1 under decreasing temperature conditions from 623K to 403K. 39
47 3.3.2 (1) s 573K 673K ε =0.8 Fig.3-4 T=623K(Fig.3-4(c)) T=673K(Fig.3-4(d)) T=523K(Fig.3-4(a) T=573K(Fig.3-4(b) ε = K MDF K, 3 10 s Fig.3-5 (Fig.3-5(a) ε =0.1 (Fig.3-5(b)) ε =0.2 (Fig.3-5(c)) ε =0.3 (Fig.3-5(d)) ε =0.5 (Fig.3-5(e)) ε =0.8, % ε =1.2 (Fig.3-5(f),(g)) 40
48 6) CA Fig.3-4 Optical microstructures evolved at ε =0.8 in single pass compression. (a) T=523K, (b) T=573K, (c) T=623K and (d) T=673K. 41
49 CA Fig.3-5 Optical microstructure changes during single pass compression at T=623K and s -1. (a) as-annealed, (b) ε =0.1, (c) ε =0.2, (d) ε =0.3, (e) ε =0.5, (f) ε =0.8 and (g) ε =
50 (2) 623K Fig.3-6 MDF 22.3µ m 6.7µ m(fig.3-6(a)) 2 3.8µ m(fig.3-6(b)) 3 1.3µ m(fig.3-6(c)) 0.8µ m (Fig.3-6(d)) 5 (Fig.3-6(e)) 403K Σε=5.4 7 TEM Fig ) 7 MDF 0.23µ m MDF Fig.3-8 Fig µ m~6.8µ m Mg 43
51 CA Fig.3-6 Optical microstructures evolved during MDF under decreasing temperature condition in Mg alloy AZ31. (a) T=623K, Σε=0.8, (b) T=523K, Σε=1.6, (c) T=493K, Σε=2.4, (d) T=473K, Σε=3.2 and (e) T=443K, Σε=
52 CA Fig.3-7 Typical TEM microstructure and the diffraction pattern of Mg alloy AZ31developed during MDF at T=403K and Σε=
53 Grain size, d / m d AZ31 = Cumlative strain, Temperature, T /K Fig.3-8 Changes in strain-induced grain size with deformation temperature during MDF of Mg alloy AZ31. Σ ε indicates the accumulated strain applied. 46
54 3.3.3 Mg 423K s -1 ( σ ε) Fig.3-9 d=22.3µ m σ ε 30% 60% MDF Mg d d=0.36µ m Mg σ ε 80% 185% (d=22.3µ m) (d=0.36µ 423K s s -1 σ ε Fig.3-10 σ ε ( ) s % s % MDF 423K 370% 5 47
55 300 AZ31 d=22.3 m T=423K = s -1 True stress, /MPa m 3.8 m 0.54 m 0.36 m Nominal strain, /% Fig.3-9 True stress-nominal strain (σ - ε ) curves at 473K and at a nominal strain rate of s -1 of Mg alloy AZ31with various grain sizes produced by MDF. 48
56 True stress, /MPa T=423K AZ31(d / m) 0.36 m 22.3 m = s s s s Nominal strain, /% Fig.3-10 Strain rate dependence of true stress-nominal strain (σ - ε ) curves for Mg alloy AZ31 with grain sizes of 0.36µ m and 22.3µ m. 49
57 3.3.4 Mg 298K s -1 σ ε Fig.4-11 (d=22.3µ m) σ ε ( σ y ) (d=0.36µ m) σ ε 526MPa 13% 1.75 ( σ p ) ( σ y = σ ) ( σ p ) ( ε u ) Fig.3-12 Fig.3-12 σ p σ y ε u 1 µ m 13% 7) (Accumulative Roll Bonding; ARB) 1100 (Al) IF 1 µ m Al IF Mg Fig.3-13 Al IF 50
58 True stress, /MPa AZ31 d=0.36 m T=298K = s m 1.2 m 6.7 m 22.3 m Nominal strain, /% Fig.3-11 True stress-nominal strain (σ - ε ) curves at 298K and at a nominal strain rate of s -1 of Mg alloy AZ31with various grain size produced by MDF. 51
59 Flow stress, y and p /MPa Uinform elongation, u % Grain size, d/ m AZ31 (a) T=298K p ( ) y ( ) ( )as-annealed ( ) ( )as-annealed Grain size, d -1/2 / m -1/2 (b) Fig.3-12 Grain size dependence of (a) flow stress and (b) uniform elongation at room temperature for Mg alloy AZ31 with various grain sizes. 52
60 Uniform elongation, u /% Grain size, d/ m T=298K Mg AZ31(hcp) Al 1100(fcc) IFSteel(bcc) Grain size, d -1/2 / m -1/2 Fig.3-13 Grain size dependence of uniform elongation at room temperature for Mg alloy AZ31, Al alloy 1100 and IF steel with various grain sizes. 53
61 1 µ m 3% 7) MDF Mg 1 µ m 13% Mg 1 µ m Al IF 1 µ m ε u 8) Mg 1 µ m Fig.4-11 σ ε Mg a a (a+c) 9) Mg MDF Mg MDF Mg AZ31 298K s -1 ( σ y = σ ) 54
62 (d) (HV(0.3)) d Fig.3-14 (( ) ( )) σ y HV(0.3) d -1/2 1/ 2 σ y = d (1) 1/ 2 H v = d (2) Fig.3-14 MDF Mg σ y HV d Hall-Petch
63 1000 Grain size, d/ m AZ31 HV(0.3) T=298K y and HV(0.3) /MPa 500 ( )As-annealed 0.23 y 0.21 ( )As-annealed Grain size, d -1/2 /m -1/2 Fig.3-14 Relationship between yield stress or hardness at 298K and grain size developed during MDF of Mg alloy AZ
64 3.4 AZ31 (MDF) (1) MDF ( ε) K MDF 1 (2) MDF 0.5Tm 403K Σ ε= µ m (3) MDF 423K s % (4) MDF 13% (5) Hall-Petch 57
65 1) : 51 (2001), ) : 51 (2001), ) X.Yang H.Miura and T.Sakai: Mater.Trans. 43 (2002), ) T.Sakai and J.J.Jonas: Encyclopedia of Materials: Science and Technology, eds. K.H.J.Buschow etal., Elseievr, Oxford, 7 (2001) ) : 52 (2002), ) Transmission Electron Microscopy: Indexing Diffraction Patterns. ed by David B.Williams and C.Barry Carter, Plenum Press New York and London (1996) ) N.Tsuji, Y.Ito, Y.Saito and Y.Minamino: Scripta Materialia, 47 (2002) ) H.Kim, S.Kang, N.Tsuji and Y.Minamino: Acta Mater., 53 (2005), ) J.Koike, T.Kobayashi, T.Mukai, H.Watanabe. M.Suzuki, K.Maruyama and K.Higashi: Acta Mater., 51 (2003),
66 ~3) 3 Mg 90 4,5) ( ) HCP 5) 4,5) 3 59
67 90 AZ mm AZ31 Table mm 21mm 14mm( 2.22:1.49:1) (Fig.2-1) 733K 7.2Ks 22.3µ m Pa 3 1 ε& = 3 10 s Fig K 90 ε 3 ε=0.8 (TEM) 200kV 0.15mm TEM, Tenupol-5 65V g 11.6g 500ml 2-n- 100ml 60
68 Fig.4-1 Schematic illustration of the thermo-mechanical p rocessing method used in multi-directional forging (MDF) with continuous decreasing temperature in each pass. WQ indicates water quenching (1) 3 623K ε& = 3 10 s 1 1 ε=0.8 - ( σ Σε) Fig.4-2 ε >0.5 61
69 True stress, /MPa AZ31 T=623K = s -1 = Cumulative strain, Fig.4-2 True stress-true strain curves of AZ31 alloy during MDF at a constant temperature of 623K and at a strain rate of s
70 (40MPa) σ Σε ( 2) K ε& = 3 10 s σ Σε Fig K σ ε Fig.4-3 ε MPa - 473K 6) 7) 473K ε < K 3.2 1/3 63
71 400 AZ s -1 True stress, /MPa T=473K (0.5Tm) Cumulative strain, Fig.4-3 True stress-true strain curves of AZ31 alloy during MDF with decreasing temperature conditions from 623K to 423K and at a strain rate of s -1. A broken curve at 473K for as-annealed sample is shown for comparison. 64
72 0.5Tm( Tm ) 423K (1) 3 623K ε& = 3 10 s 1 Fig.4-4 Fi.4-4(a),(b),(c),(d) ε = ε = 0. 8 (Fig.4-4(a)) 6.7µ m µ m (Fig.4-4(b),(c),(d)) Mg (2) 623K 423K Fig.4-5 Fi.4-5(a),(b),(c),(d) ε = (Fig.4-5(a)) 22.3 m 6.7 m(fig.4-5(b)) m(fig.4-5(c)) 65
73 CA Fig.4-4 Optical microstructures evolved in AZ31 alloy during MDF at a constant temperature of 623K. (a) Σε=0.8, (b) Σε=1.6, (c) Σε=2.4 and (d) Σε=
74 CA Fig.4-5 Optical microstructures evolved in AZ31 alloy during MDF with continuous decreasing temperature in each p ass. (a) As annealed, (b) T=623K, Σε=0.8, (c) T=523K, Σε=1.6, and (d) T=473K, Σε=
75 0.8 m (Fig.4-5(d)) 623K 1 - (Fig.4-3) (Fig.4-5(b)) 4,5), HCP 5) HCP,, 8) 473K 1/3 4) 4,7) 68
76 K ε = K ε = TEM Fig.4-6(a),(b) 9) - T=453K ε = µ m T=423K ε = µ m 403K ε = m (Fig.4-6(c)) ECAE(Equal-Channel Angular Extrusion) AZ31 473K ε 8. 0 (8 ) 1.1 m 10) 453K ε = 4. 0 (5 ) 0.54 m 69
77 CA 70
78 CA Fig.4-6 Typical TEM microstructures and the diffraction p atterns of AZ31 alloy evolved during MDF. (a) T=453K and Σε=4.0, (b) T=423K and Σε=4.8 (c) T=403K and Σε=
79 Fig.4-7 TEM 473K (Fig.4-3) 423K Σ ε = MPa, 0.36µ m 0.1µ m 0.1µ m Fig.4-7, Fig MPa 2 N, σ = k D, N 100MPa 0.90 N 0. 2 Fig.4-7 N 0.75 N ) σ D 72
80 500 AZ31 a Steady state stress, / MP OM TEM MDF One-pass compression Grain size, d / m Fig.4-7 Relationship between flow stress and grain size developed during MDF and single-pass compression. 73
81 4.4.2 Fig.4-8 (Fig4-8(a)) EBSD Σε = 0. 8 (Fig.4-8(b) (f)) TEM (2.6.4 ) TEM EBSD EBSD TEM 51 (Fig.4-8(a)) Σε = 0. 8 Σε = (Fig.4-8(b)) 34 (Fig.4-8(c)) Σε = 3. 2 θ =38 (Fig.4-8(d)) Σ ε = θ =49 (Fig.4-8(e)) 6 ( Σε = 4. 8 ) 50 (Fig.4-8(f)) ( Σε = 0. 8 ) 74
82 0.3 (a) AZ31 =0 (b) =0.8 cy, f Frequen =51 - = (c) =1.6 0 (d) =3.2 Frequency, f =34 - = (e) =4.0 0 (f) =4.8 Frequency, f =49 - = Misorientation, /deg Fig.4-8 Misorientation distributions of (sub) grain boundaries developed in MDF. 75
83 4.5 AZ31 (1) 473K 0.5Tm 423K (2) 423K Σ ε = µ m 403K Σ ε = µ m (3) 100MPa N 2 σ = k D <100Mpa N 0.9, >100MPa N 0.2 (4)
84 1) B.L.Mordike and T.Ebert: Material Science and Engineer A. 302 (2001), 37 2) : 51 (2001), ) : 51 (2001), ) : 52 (2002), ) X.Yang, H.Miura, T.Sakai: Materials Science Forum, (2003), ) T.Sakai and J.J.Jonas: Encyclopedia of Materials: Science and Technology, eds. K.H.J.Buschow etal., Elseievr, Oxford, 7 (2001) ) J.Koike, R.Ohyama, T.Kobayashi, M.Suzuki and K.Maruyama: Mater. Trans. JIM 44 (2003), ) (2003), ) A.Belyakov, T.Sakai, H.Miura and R.Kaibyshev: Philozophical Magazine Letters, 80 (2000), ) Lawrence CISAR 52 (2002) ) A.Belyakov, T.Sakai, H.Miura, and K.Tuszaki: Philosophical Magazine A, 81 (2001),
85 5 5.1 (Mg) 1) 3 4 Mg AZ31 (MDF) Mg MDF Mg AZ mm Mg AZ31 Table mm 21mm 14mm( 2.22:1.49:1) (Fig.2-1) 773K 7.2ks 22.3µ m (Fig.4-5(a) ) Pa 623K 78
86 90 ε=0.8 MDF 3 1 ε& = 3 10 s 423K ( Σ ε) µ m 2) 3mm 6mm 0.7mm R 1mm MDF L-ST (TA) (CA) (Fig.5-1) CA 14 R=1 3 6 ST LT TA L Fig.5-1 Tensile specimens machined parallel to L-ST plane of MDFed Mg alloy. The tensile axis (TA) was perpendicular to the final compression axis (CA) Pa 373K 473K s ks 79
87 (OM) (OIM) (SEM/EBSD) MDF Mg ( σ ε ) 373K 423K 473K Fig.5-2 ε σ ( σ ) ε ) Fig.5-3 ( s -1 ) p σ ε 100% 100% 300% 393K s % ( n = 1/ m = ln & ε / lnσ ) n 3 200% n = 5.0 ~ 6.3 ( T 3-5) Fig.5-3(a) n > 5 200% 10-3 s -1 n 80
88 = s 1 AZ31 T=393K True stress, /MPa 100 = s 1 = s 1 = s Nominal strain, /%
89 200 = s 1 AZ31 T=423K True Stress, /MPa 100 = s 1 = s Nominal Strain, /%
90 True stress, /MPa AZ31 T=473K = s 1 = s 1 = s Nominal strain, /% 400 Fig.5-2 Strain rate dependence of true stress-nominal strain ( σ - ε ) curves. (a) 393K, (b) 423K and (c) 473K. 83
91 Peak Flow Stress, p /MPa AZ31 n =5.6 (a) n 1 Elongation, T (%) T=393K T=423K T=473K (b) Strain Rate, /s Fig.5-3 Strain rate dependence of (a) peak flow stress σ p and (b) total elongation to fracture ε T of MDFed Mg alloy tested at 393K, 423K and 473K. 84
92 5.3.2 (1) 473K s -1 (Fig.5-1 L-ST ) Fig.5-4 (a) (b)40% (c)100% (d) 350% MDF 0.36µ m 2.2µ m (Fig.4(a)) 40% 3.6µ m 100% 4.6µ m 350% 4.1µ m 473K (Fig.5-1 L-ST ) Fig.5-5 (Fig.5-5(a)) s -1 (Fig.5-5(b)) s -1 (Fig.5-5(c)) s -1 (Fig.5-5(d)) Fig s -1 Fig s % 2.5µ m s µ m 85
93 TA L ST Fig.5-4 Optical microstructures developed in MDFed Mg alloy during tensile deformation at 473K and at s -1. (a) ε =0%, (b) ε =40%, (c) ε =100%, and (d) ε 350%. 86
94 TA L ST Fig.5-5 Changes in grained structure developed at ε 100% with strain rate at a temperature of 473K. (a) Before deformation (ε =0%), (b) s -1, (c) s -1, (d) s
95 TA L ST Fig.5-5 Changes in grained structure developed at ε 100% with strain rate at a temperature of 473K. (a) Before deformation (ε =0%), (b) s -1, (c) s -1, (d) s
96 Grain Size, d/ m AZ31 T=473K = s -1 = s -1 = s -1 ( )As-MDFed Nominal Strain, /% Fig.5-6 Effect of strain rate on changes in average grain size with tensile deformation at 473K. 89
97 µ m (1) Mg (2) (2) SEM/EBSD 473K s % (OIM) Fig.5-7 (Fig.5-1 ST ) θ =2 4 θ =4 15 θ>15 ( ) Fig.5-7 MDF Mg hcp {0001} (TA) {0001} //TA (Fig.5-7(a)) 350% (Fig.5-7(b)) 90
98 LT L TA Fig.5-7 OIM micrographs and inverse pole figures developed in L-LT plane of MDFed Mg alloy deformed in tension at 473K and at s -1. (a) ε =0% and (b) ε 350% 91
99 µ m 6-8) p n ε& = k d σ exp( Q / RT ) (5-1) k p n Q R ε& T (5-1) k d p / n σ = 1 (5-2) k 1 (Fig.5-6) σ p d σ Fig.5-8 p p σ d N σ k d (5-3) p = 2 k N = n Fig.5-3 n' & ε = k3 σ P (5-4) (5-4) n Fig.5-3(a) n'= 5.0 ~
100 Peak Flow Stress, p /M Pa N=0.9 AZ31 T=473K Grain Size, d/ m Fig.5-8 Relationship between peak flow stress σ P and grain size d developed in high strain for MDFed Mg alloy tested at 473K. 93
101 n n' (5-2) (5-3) (5-4) n n p N p n = n + (5-5) N p ) N = 0.9 n '= 5.0 ~ 6. 3 p =2 3 (5-5) n n = 2.8 ~ 3. 0 n 3 σ & ε Fig.5-9 P σ & ε Fig.5-9 P n 3 d 1 > d 2 > d 3 n'= 5.0 ~
102 Pa Peak Flow Stress, p /M AZ31 T=473K n'=5.6 n=3.0 d 1 =4.6 m d d 1 d 2 d 2 =2.5 m 3 d 3 =1.9 m Strain Rate, /s -1 Fig.5-9 Schematic drawing of predicted strain rate dependence of p eak flow stress (broke line) and the experimental data at 473K. 95
103 5.4.2 MDF Mg Fig K s -1 LT ST L SEM/EBSD Mg 10) Mg Mg hcp { 0001} 473K s -1 5% 40% (L-ST ) OIM Fig.5-11 SEM/EBSD Fig.5-11 (Fig.5-11 a,b,c,d) 5% 40% Fig.5-11(a),(b) a,b,c,d 96
104 Elongation Surface 0% 350% L-LT Max=3.2 Max=3.0 L-ST Max=1.6 Max=1.7 LT-ST Max=2.1 Max=2.2 Fig.5-10 Inverse pole figure and maximum intensity of the texture in L-LT, L-ST and LT-ST plane for MDFed Mg alloy deformed in tension at 473K and at s
105 ST L TA Fig.5-11 OIM micrographs in L-LT surface at a same place during tensile deformation at 473K and at s -1. (a) ε =5% and (b) ε =40% 98
106 5 10 Fig5-11 c d L-ST 5% 40% Mg Mg 99
107 5.5 Mg 1. n s % 370% σ d ( n 3 ) n > 5 4. {0001} 350% 5. Mg 100
108 1) : 51 (2001), ) J.Xing, H.Soda, X.Yang, H.Miura and T.Sakai: Mater. Trans., 46 (2005), ) R.H.Bricknell and J.W.Edington: Mater. Trans., 7A (1976) ) K.Higashi, M.Mabuchi and T.G.Langdon: ISIJ Intl.36 (1996) ) T.G.Langdon: Mater. Sci. Eng., A174 (1994) ) T.G.Nieh, J.Wadsworth and O.D.Sherby: Superplasticity in metals and ceramics,(cambridge University Press, 1997) ) 29 (1990), 22. 8) N.Ridley: Mater.Sci.Tech, 6 (1990), ) J.W.Edington, K.N.Melton and C.P.Cutler: Prog. Mater. Sci., 21 (1976), ) X.Yang, H.Miura and T.Sakai: Mater Trans., 43 (2002)
109 6 6.1 (Mg) 1) 3 4 Mg AZ31 (MDF) 5 Mg MDF Mg AZ Mg mm Mg AZ31 60mm 40mm 27mm( 2.22:1.49:1) 773K 7.2ks 33.6µ m Mg 102
110 s K 423K MDF ( Σε=4.8) 0.43µ m (Fig.6-1) 4mm 10mm 1mm R 1mm (Fig.6-2) (0 ) hcp { 0001} (TA) ( 5 ) 45 (45 ) (90 ) 2 hcp { 0001} TA 45 MDF L ST LT 45 45L K s -1 SEM/EBSD 103
111 CA 1 µ m Fig.6-1 Typical TEM microstructure of AZ31 alloy MDFed to Σε=4.8at T=423K. 90 TA 45 CA 0 R t=1 (a) 45L L ST LT (b) TA Fig.6-2 (a) Tensile test specimens with the angles of inclination of 0, 45 and 90 against the final compression axis (CA) of MDFed Mg alloy. (b) Dimension of tensile sample in mm. 104
112 K s -1 ( σ ε) Fig.6-3 σ ε ( σ P ) ( ε T ) ( n = 1/ m = ln & ε / lnσ ) Fig.6-4 Fig.6-3, s % s MPa 100% MPa 137MPa 68% 82% s MPa 200% MPa 58MPa 320% 280% Mg 105
113 True stress, /MPa (a) AZ31 T=423k = s Nominal strain, /%
114 200 AZ31 T=423K (b) True stress, /MPa = s Nominal strain, /%
115 200 AZ31 T=423K (c) True stress, /MPa = s Nominal strain, /% 350 Fig.6-3 Effect of the anisotropy of MDFed AZ31 alloy on σ ε curves at 423K. (a) ε& = 5 10 s, (b) ε& = 5 10 s, 5 1 and (c) ε& = 5 10 s. 108
116 Total elongation, T (%) Peak flow stress, P /MPa 300 T=423K n=4.9 1 n (a) (b) Strain rate, /s -1 Fig.6-4 Strain rate dependence of (a) peak flow stress and (b) total elongation of MDFed AZ31 alloy. 109
117 6.3.2 SEM/EBSD hcp {0001}// (TA) 0 2) K s % (Fig L LT ) OIM 200% Fig % (Fig.6-2 L ST ) (OIM) 200% Fig.6-6 θ =2 4 θ =4 15 θ>15 ( ) Fig.6-5(a),6-6(a) OIM TA hcp % Fig.6-5(b),6-6(b) OIM { 0001} % 200% hcp { 0001} TA
118 45L LT TA Fig.6-5 OIM micrographs and inverse pole figures developed in longitudinal section parallel to TA of 45 sample deformed in tension at 473K and at s -1. (a) ε =5% and (b) ε =200% 111
119 L ST TA Fig.6-6 OIM micrographs and inverse pole figures developed in L-LT plane of 0 sample deformed in tension at 473K and at s -1. (a) ε =5% and (b) ε =200% 112
120 0 MDF { 0001} TA (Fig.6-7 ) { 0001} TA 45 (Fig.6-5(a),6-6(a)) { 0001} 200% TA (Fig.6-5(b),6-6(b)) (Fig.6-4(c)) 6.4 Fig.6-3,4 ( σ P ) ( ε T ) Fig s -1 0 σ P σ P (Fig.6-8(a)) σ P s -1 σ P 200% s % 0 200% σ P { 0001} MDF 0 { 0001} TA TA
121 Sample Initial Large elongation 0 45, 90 Fig.6-7 Texture changes taking place in 0, 45 and 90 samples during tensile deformation. 114
122 Peak floe stress, P /MPa (a) AZ31 T=473K s s s -1 Elongation, f / % (b) s s s Angle to L direction, /degree Fig.6-8 Effect of the anisotropy of MDFed AZ31 alloy on (a) peak flow stress and (b) total elongation. A main texture { 0001} was developed roughly parallel to L-LT p lane. 115
123 (Fig.6-5(a),Fig.6-6(a)) Texture hardening / softening s ε& < 10 s n 4 σ P 200% s % { 0001} 45 { 0001} Texture hardening (Fig.6-3(c)) 3) 2 Al 4) Mg 116
124 5) Mg Fig.6-9 Gifkins 6) { 0001} { 0001} s % 117
125 Grain boundary dislocation pile up N ew dislocations in grain boundaries and grains Basal sliding dislocations Fig.6-9 Gifkins model for grain boundary sliding due to dislocation motion 6). 118
126 6.4 MDF Mg AZ K s % % n 4 3. hcp Mg 3 119
127 1) : 51 (2001), ) : 56 (2006), No12 3) J.W.Edington, K.N.Melton and C.P.Cutler: Progress in Materials Science, 21 (1976), 61. 4) K.Matsuki, N.Hariyama, M,Tokizawa and Y.Murakami: Metal.Sci., 17 (1983), ) H.Watanabe, T.Mukai, M.Kohzu, S.Tanabe and K.Higashi: Acta Mater., 47 (1999), ) R.C.Gigkins: Metal Trans. A, 7A (1976),
128 7 (Mg) (hcp) Mg Mg 90 (Multi-Directional Forging, MDF) Mg AZ31 MDF MDF Mg MDF 1 Mg 2 121
129 3 Mg AZ31 623K MDF Mg MDF 423K 300% Hall-Petch 0.36µ m 10% Mg 4 Mg AZ s K 403K MDF MDF 122
130 403K Σε= µ m 5 MDF Σε=4.8(6 ) 0.36µ m 6mm 3mm 0.7mm 10-3 s % 370% Mg 6 MDF Mg (90 ) 45 (45 ) (0 ) MDF Mg hcp (0 ) hcp (45 90 ) 123
131 0 Mg MDF =0.8 ( 3 ) ( 5 6 ) Mg MDF Mg MDF ( 6 ) 124
132 7 125
133 (1) 邢 AZ31 54 (2004), (2005 ) ( 4 ) (1) Jie Xing, Hiroshi Soda, Xuyue Yang, Hiromi Miura and Taku Saki: Ultra-Fine Grain Development in an AZ31 Magnesium Alloy during Multi-Directional Forging under Decreasing Temperature Conditions, Materials Transactions, 46 (2005), ( 4 ) (2) Jie Xing, Xuyue Yang, Hiromi Miura and Taku Saki: Grain Refinement in Magnesium Alloy AZ31 during Multidirectional Forging under Decreasing Temperature Conditions, Materials Science Forum, (2005), ( 4 ) (3) Xuyue.Yang, Jie.Xing, Hiromi.Miura and Taku.Sakai: Strain-Induced Grain Refinement of Magnesium Alloy AZ31 during Hot Forging, Materials Science Forum, (2006), ( 3,4 ) (4) 邢 AZ31 56 (2006) () ( 5 ) (4) Jie Xing, Xuyue Yang, Hiromi Miura and Taku Saki: 126
134 Superplasticity of Fine-Grained Magnesium Alloy AZ31 Processed by Severe Plastic Deformation, Materials Transactions, 48 (2007), () ( 5 ) (5) Jie Xing, Xuyue Yang, Hiromi Miura and Taku Saki: Low Temperature Superplasticity of Fine-Grained Magnesium Alloy AZ31, Advanced Materials Research, (2007), ( 5 ) (6) AZ31 ( ) 3 ( ) 127
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