摩擦攪拌プロセスの攪拌効果と温度履歴を利用した熱処理型アルミニウム合金鋳物の改質 利用統計を見る

1

... 1

1.1

... 1

1.1.1

... 1

1.1.2 AC4CH

... 3

1.1.3 AC4CH

... 7

1.1.4

... 11

1.1.4.1

... 11

1.1.4.2

... 13

1.2

... 15

... 19

2

... 23

2.1

... 23

2.1.1

... 23

2.1.2

... 24

2.2

... 25

2.3

... 36

2.4

... 41

2.4.1

... 41

2.4.2

... 47

2.4.3

... 50

2.5

... 53

2.5.1

... 53

2.5.1.1

... 53

2.5.1.2

-Al

Mg

Si

... 58

2.5.1.3

... 61

2.5.1.4

Si

... 65

2.5.2

... 66

2.5.2.1

... 66

2.5.2.2 Mg

Si

... 68

2.5.2.3

Si

... 71

2.6

Si

... 74

2.6.1

Si

... 74

2.6.2

... 88

2.7

... 95

2.8

... 98

1

... 98

... 99

3

Si

... 102

3.1

... 102

3.1.1

... 102

3.2

... 102

3.3

... 107

3.3.1 ECAP

... 107

3.3.2

Si

... 111

3.3.3

Si

... 121

3.4

... 135

3.5

... 136

1 ECAP

Si

... 136

... 143

4

.. 144

4.1

... 144

4.1.1

... 144

4.2 FSP

... 144

4.2.1 FSP

... 145

4.2.2 FSP

... 146

4.2.3

... 150

4.2.3.1

... 150

4.2.3.2

... 153

4.2.4

... 169

4.2.4.1

... 169

4.2.4.2

... 171

4.2.5

... 177

4.3 FSP

... 178

4.3.1

... 178

4.3.2

... 179

4.3.2.1

... 179

4.3.2.2

... 182

4.3.3

... 190

4.4

... 191

4.5

... 192

... 194

5

... 195

... 202

... 203

1

1 . 1

1 . 1 . 1

100 1)2) ! 1/3 ! (Al-Zn-Mg-Cu ) ! ! ! 60% 2 ! 3 !

! ! 3% CO2 2 (2011 )3) 9 (2011 )4) 5) 8 6) ① ② ③ ④ 6) 8) 9) 11)

1 . 1 . 2

A C 4 C H

AC4CH ( AC4CH ) Al-Si Mg Fe 1 . 1 JIS AC4CH Mg Mg2Si Fe Fe AC4CH 9),12) 1 . 1 AC4CH (JIS ) AC4CH

α-Al (Al) α-Al

(Al) Si Fe Mg2Si AC4CH ( µm µm ) ① ② ③ 13) 22) Si ( µm µm )

Al-Si2 557 12.6(mass% mass%

) Si 1.65% (577 )

23) _{Si Si Si (}

) 24) 29)

30) _Si Si 31) _{Na Sr Sb} 32)33) Si Si ( µm ) AC4CH -Al

2 (Dendrite Arm Spacing DASⅡ ) -1/3

12) _DASⅡ 12),31) Fe ( µm µm ) Fe 0.03 0.05%(655 ) 34) Fe 35) _Fe Si 36) ( nm nm ) AC4CH ( -Al ) Mg2Si (β”) AC4CH 1 . 2 Si Fe

1 . 1 A C 4 C H ( m a s s % ) Si Fe Cu Mn Mg Zn Ni Ti Pb Sn Cr Al JIS 6.5- -0.2 -0.1 -0.1 0.25- -0.1 -0.05 -0.2 -0.05 -0.05 -0.05 bal. AC4CH 7.5 0.45 1 . 1 A C 4 C H

10µm

50µm

α-Al

Si

100µm

α-Al

10µm

Fe

1 . 2 A C 4 C H

α-Al

Si

Fe

! 

(

)

! 

Si

Fe

! 

Si

Fe

! 

Si

Fe

1 . 1 . 3 A C 4 C H

( ) ( ) 37),38) 39) 44) ! AC4CH AC4CH Mg Si Al-Mg2Si 2 1 . 3 Al-Mg2Si 2 -Al Mg2Si 595 1.85% Mg2Si AC4CH 1 . 4 (T6) (Mg Si) (Al) Si ( ) Mg Si Mg2Si ( ”) AC4CH 535 12) Si Si 45) 50) Si

Zhang 47) _A356 (JIS:AC4CH ) 505 30s 550 30min 6h 95% 49) _AC4CH Al-Si-Mg 560 30min 540 300min 16% 1 . 3 A l - M g2S i 2

Al

Mg

₂

Si (mass%)

Tem

per

at

u

re

, T

/

0

100

200

300

400

500

600

700

L

L+(Al)

(Al)

1.85%

595

13%

(Al)+Mg

₂

Si

2

4

6

8

10 12 14

1 . 4 A C 4 C H

!

ECAP(Equal-Channel Angular Pressing ECAP )51) _{ARB(Accumulative}

Roll-Bonding ARB ) 52) _{(Friction Stir Processing FSP}

)53)

ECAP(Equal-Channel Angular Pressing)

ECAP 1 . 5 54),55) _ECAP ECAP -Al Si 56),57) _{AC4CH ECAP Si} 58)

1 . 5 E C A P

ARB(Accumulative Roll-Bonding) ARB 1 . 6

52) _Jamaati 59) _{A356 ARB ARB}

ARB Si 1 . 6 A R B

Φ

Channel

ECAP die

ψ

Specimen

Cutting Stacking Roll bonding

Specimen

FSP(Friction Stir Processing) FSP

15 25

47)

ECAP ARB FSP AC4CH

-Al Si Si 17) 28) 31) Si Si Si

1 . 1 . 4

1 . 1 . 4 . 1

(Friction Stir Processing FSP )53) _{1991 TWI(The}

Welding Institute of the United Kingdom) (Friction Stir Welding

FSW )60) _{1 . 7 FSP(}

FSW) FSP

FSP ( )

( 1 . 7 - 1 ) ( 1 . 7 - 2 )

( 1 . 7 - 4 ) 1 . 8 FSP( FSW)

(Stir Zone) µm

(Thermo Mechanically Affected Zone TMAZ)

(Heat Affected Zone HAZ) 61) _FSP

1 . 7 F S P

1 . 8 F S P ( o r F S W )

1 . 1 . 4 . 2 FSP

62)

FSP 1 . 9

Al-Cu-Si AC2B Al-Si-Mg AC4C Al-Si-Cu

ADC12 63) 68)

AC4CH (A356 ) AC4CH

(A356 ) Sharma 69) _FSP FSP Si 80% Ma 70) _FSP α-Al 3µm Santella 71) _FSP FSP Ma 72) 73) _FSP (T6 ) Si Al Si FSP FSP FSP FSP 74) 74) _FSP FSP 75) FSP Si 2 -Al FSP FSW

76) 84) _Y.S.Sato77) _{A6063 (Al-Mg-Si ) T5}

FSW ( )

FSP(FSW) 85) _FSP 86) FSP(FSW) FSP FSP ( ) FSP ( ) Al FSP 1 . 9 F S P

AC2B

Alloy

Year

2000

2005

63)

FSP

2010

AC4C

AC4CH

(A356)

A319

ADC12

64)

FSP

) 73) 68)

Santella

)

Sharma

69)

Ma

70) 66)

FSP

Nakata

67)

FSP

Ma

)

Ma

)

FSP

Ma

)

FSP

Santella

)

1 . 2

AC4CH FSP 1 . 1 0 FSP ( ) Si FSP FSP FSP FSP FSP 2 FSP FSP 2 FSP AC4CH FSP ( /s) 87) _FSP FSP ( /s) FSP FSP FSP 2 3 AC4CH

2 4 2 5 Mg Si Si 2 6 Si Si 3 FSP Si AC4CH AC4CH -Al Si Si Si Si Si FSP Si ECAP Si Si Si 4 FSP FSP FSP FSP FSP

FSP FSP FSP FSP (4.2 ) FSP Mg Si FSP (4.3 ) (4.4 ) FSP

2 2.3 2.4 2.5 2.6 Si 3 Si !  Si !  Si

AC4CH

!  !  ( ) !  Si Fe !  Si Fe Si ECAP ARB FSP 4 4.3 FSP 4.4 4.2 FSP

1.10

1) http://www.aluminum.or.jp/basic/aluminumtoha/fset1.html (2013 9 ) 2) 6 ( ) (2001) pp.2. 3) http://www.mlit.go.jp/sogoseisaku/environment/sosei_environment_tk_000006.html (2013 9 ) 4) http://www.mlit.go.jp/sogoseisaku/environment/sosei_environment_tk_000007.html (2013 9 ) 5) http://www.mlit.go.jp/common/000989167.pdf (2013 9 ) 6) R D , Vol.57,No.2 (2007), pp.2-7. 7) Vol.58 No.6 (2008) pp.259-273. 8) pp.59. 9) Vol.57 No.7 (2007) pp.331-333. 10) Vol.57 No.7 (2007) pp.334-335. 11) Vol.59 No.3 (2009) pp.148-153. 12) Vol.61 No.9 (2011) pp.485-503. 13) Vol.55 No.12 (1983) pp.742-750. 14) Vol.39 No.3 (1989) pp.203-209.

15) C.H.Caceres B.I.Sellong Mater. Sci. Eng. A220 (1996) pp.109-116.

16) Vol.70 No.4 (1998) pp.254-259.

17) A.M.Gokhale G.R.Patel Mater. Chara. Vol.54 (2005) pp.13-20.

18) J.A.Francis G.M.Delphine Cantin Mater. Sci. Eng. A407 (2005) pp.322-329. 19) A.M.Gokhale G.R.Patel Scr. Mater. Vol.52 (2005) pp.237-241.

20) G.Ran J.Zhou Q.G.Wang J. Alloys Compo. 421 (2006) pp.80-86. 21) C.D.Lee Mater. Sci. Eng. A464 (2007) pp.249-254.

22) X.Teng Y.Bai T.Wierzbicki Vol.57 No.9 (2008) pp.913-920.

23) 40 ( ) (1991)

24) Vol.19 No.9 (1969) pp.398-408.

25) Vol.20 No.5 (1970) pp.247-255.

26) Vol.30 No.3 (1980) pp.147-153.

27) M.F.HAFIZ Vol.43 No.9 (1993) pp.472-477.

28) Q.Lihe Vol.55 No.2 (2005)

pp.75-81. 29) Vol.60 No.1 (2010) pp.7-11. 30) Vol.41 No,6 (1991) pp.398-405. 31) Vol.37 No.4 (1987) pp.268-275. 32) Vol.34 No.6 (1984) pp.361-373. 33) Vol.37 No.2 (1987) pp.146-152. 34) 40 ( ) (1991) pp.341 35) No.5 (1940) pp.1-27. 36) Vol.83 No.1 (2011) pp.47-57. 37) Vol.76 No.4 (2004) pp.266-271. 38) 6 ( ) (2001) pp.200. 39) http://www.j-imono.com/column/daredemo/22.html (2013 9 ) 40) Vol.76 No.4 (2004) pp.283-288. 41) Vol.39 No.7 (1989) pp.487-493.

42) C.Park S.Kim Y.Kwon Y.Lee J.Lee Mater. Sci. Eng. A391 (2005) pp.86-94.

43) Vol.56 No.1 (2006) pp.21-27.

44) S.Tahamtan M.A.Golozar F.Karimzadeh B.Niroumand Mater. Chara. Vol.59(2008) pp.223-228

45) Vol.45 No.8 (1995) pp.447-452.

46) Vol.68 No.10 (1996) pp.891-897.

47) D.L.Zhang L.H.Zheng D.H.StJohn J.Light Metals 2 (2002) pp.27-36 48) S.K.Chaudhury L.Wang D.Apelian AFS Transactions (2004) pp.289-304

49) Vol.55 No.4 (2005) pp.159-163.

51) V.M.Segal V.I.Reznikov A.E.Drobyshevskiy V.I.Kopylov Russian Metallurgy-Metally Vol.1 (1981) pp.115-119.

52) Y.Saito H.Utsunomiya N.Tsuji T.Sakai Acta Mater. Vol.47 (1999) pp.579-583. 53) R.S.Mishra M.W.Mahoney S.X.McFadden N.A.Mara A.K.Mukherjee Scripta Mater., Vol.42

(2000) pp.163-168.

54) Terence G. Langdon Vol.37 No.9 (1998) pp.767-774.

55) R.Z.Valiev Y.Estrin Z.Horita T.G.Langdon M.J.Zehetbauer Y.T.Zhu JOM Vol.58 No.4 (2006) pp.33-39.

56) A.Ma N.Saito M.Takagi Y.Nishida H.Iwata K.Suzuki I.Shigematsu A.Watazu Mater. Sic. Eng. A395 (2005) pp.70-76.

57) I.gutierrez-Urrutia M.A.Munoz-Morris D.G.Morris Acta Mater. Vol.55 (2007) pp.1319-1330.

58) Y.Nakayama T.Miyazaki Mater. Trans. Vol.52 No.11 (2011) pp.2045-2051.

59) R.Jamaati S.Amirkhanlou M.R.Toroghinejad B.Niroumand Mater. Sci. Eng. A528 (2001) pp.2495-2501.

60) -FSW - ( ) (2006) pp.12.

61) -FSW - ( ) (2006) pp.15.

62) R.S.Mishra Z.Y.Ma Mater. Sci. Eng. R50 (2005) pp.1-78.

63) Vol.49 No.12 (1999) pp.607-612.

64) Vol.53 No.1 (2003) pp.15-19.

65) Vol.53 No.10 (2003) pp.405-409.

66) Vol.78 No.9 (2006) pp.451-456.

67) K.Nakata,Y.G.Kim,H.Fujii,T.Tsumura,T.Komazaki : Mater. Sci. Eng.,A437 (2006) pp.274-280.

68) Vol.30 No.2 (2012) pp.180-187.

69) S.R.Sharma Z.Y.Ma R.S.Mishra : Scripta Mater., Vol.51, (2004) pp.237-241. 70) Z.Y.Ma R.S.Mishra M.W.Mahoney : Scripta Mater., Vol.50 (2004) pp.931-935.

71) M.L.Santella T.Engstrom D.Storjohann T.Y.Pan : Scripta Mater., Vol.53 (2005) pp.201-206.

72) Z.Y.Ma S.R.Sharma R.S.Mishra Mater. Sci. Eng. A433 (2006) pp.269-278.

73) Vol.58 No.1 (2009)

74) Z.Y.Ma S.R.Sharma R.S.Mishra Metal. Mater. Trans. A Vol.37A (2006) pp.3323-3336. 75) Z.Y.Ma S.R.Sharma R.S.Mishra Scripta Mater., Vol.54 (2006) pp.1623-1626.

76) L.E.Murr G.Liu J.C.McClure J. Mater. Sci. (1998) pp.1243-1251.

77) Y.S.Sato H.Kokawa M.Enomoto S.Jogan Metal. Mater. Trans. A Vol.30A (1999) pp.2429-2437.

78) Y.S.Sato H.Kokawa M.Enomoto S.Jogan T.Hashimoto Metal. Mater. Trans. A Vol.30A (1999) pp.3125-3130.

79) K.V.Jata K.K.Sankaran J.J.Ruschau Metal. Mater. Trans. A Vol.31A (2000) pp.2181-2192. 80) B.Heinz B.Skrotzki Metal. Mater. Trans. B Vol.33B (2002) pp.489-498.

81) J.-Q.Su T.W.Nelson R.Mishra M.Mahoney Acta Mater. Vol.51 (2003) pp.713-729. 82) R.W.Fonda J.F.Bingert Metal. Mater. Trans. A Vol.35A (2004) pp.1487-1499.

83) Vol.25 No.4(2007)

pp.553-559.

84) A.Goloborodko Vol.60

No.6 (2010) pp.275-281.

85) Vol.56 No.3 (2006) pp.162-165.

86) Kh.A.A.Hassan A.F.Norman D.A.Price P.B.Prangnell Acta Mater. Vol.51 (2003) pp.1923-1936.

87)

2

2.1

FSP FSP FSP

2.1.1

1 (535 ) 15 25 1) 4) NaOH 2.1.1 FSP 5) _FSP

IH 6) 8) 9) 40 400kHz 2000kHz FSP 2.1.1

2.1.2

FSP FSP ( )

Target holding temp.

Tem

p.

time

Electrical furnace

Salt-bath

&

Fluid bed

Induction

heating

Overheat

2.3 2.4 2.5 Mg Si Si 2.6 Si Chaudhury 10) _{AC4CH Mg D357} Si Al Si Si Si Si

2.2

! AC4CH (JIS ) Ar Sr Si 700 150 ( ) 2.2.1 2.3 2.4 2.5 2.2.1 10mm 10mm 50mm 2.3 2.4 2.5

( c,d ) ( a,b ) 2.5 (2.5.1.1) 2.6 2.2.2 10mm 5mm 2.2.1 AC4CH (mass%) Si Fe Cu Mn Mg Zn Ni Ti Pb Sn Cr Sr(ppm) Al Sample 6.9 0.12 <0.01 <0.01 0.37 0.01 <0.01 0.13 <0.01 <0.01 <0.01 48 bal. 2.2.1 2.2.2

a

b

c

d

3mm

_20mm

Ingot

190mm

22mm

50mm

10mm

10mm

20mm

Ingot

190mm

22mm

5mm

Φ

10mm

! 2.2.3 2.2.2 2.2.3 2MHz 2.2.4 ( ) 2.2.5 2 ( ) ( ) 2.3 2.4 2.5 2.6 2.2.4 20 ( 2.2.4 ) 2.2.3

A

B

H

C

D

E

F

G

2.2.2 2.2.3 2.2.4 ( )

A

ORION

(RKE1500A-V)

B

C

(IGA C-E1)

D

E

(SH-7A-64)

F

G

H UNIT COOLER

ORION

(RKS750S)

(Hz)

2M

(W)

10k

Heating coil

Specimen

Radiation thermometer

Water bath

(20 )

2.2.5 ( ) 2.2.4 Heating coil Specimen (10mm×10mm×50mm) Heating coil Specimen (Φ10mm×5mm)

IGA C-E1

( )

250 2000

(µm)

1.6

InGaAs

! 2.4 2.2.6 2.4.1 ( 40.0 /s) 450 570 0min 20 48 T4 AC4CH (T6 ) T4 2.4.2 2.4.3 2.5 2.6 T4 2.4.2 40.0 /s 560 0 3 10 30min 4 2.4.2 560 30min 0min 30min 2.4.3 560 3min 40.0 4.0 0.4 /s 3 2.5 2.2.7 ( 2.2.1 c,d ) 40.0 /s 560 0min 30min 20 2.5.1.1 Mg ( 2.2.1 a,b ) 40.0

/s 560 0min 7min 1min 20

(

535 8h)

Si 2.6 2.2.8 90.0 /s

0.9 /s 2 560 0,3,10 30min 4

2.2.6 2.4

2.2.7 2.5

2.4.1 Study on solution temp. 2.4.2 Study on solution time

2.4.3 Study on heating rate

Tem p. Time 48h at R.T. Temp. : 560 W.Q. at 20 Holding time : 0,3,10 and 30min Heating rate : 40.0 /s Holding time : 0min

Tem p. Time 48h at R.T. W.Q. at 20 Temp. : 450 570 Heating rate : 40.0 /s Tem p. Time 48h at R.T. W.Q. at 20 Heating rate : 40.0 4.0 0.4 /s Holding time : 3min

Temp. : 560

a

b

Tem

p.

Time

48h at

R.T.

Temp. : 560

W.Q. at 20

Holding time :

0,3,10 and 30min

Heating rate : 40.0

/s

Heating rate : 40.0 /s

W.Q. at 20

_{48h at}

R.T.

Holding time :

0 to 7min

c

d

Ingot

2.2.8 2.6 ! Si 2 (Optical Microscope OM ) USB (L-830) ( 25mm 25mm ) 2.2.5 2.2.5

Tem

p.

Time

48h at

R.T.

Temp.:

560

W.Q. at 20 W.Q. at 20

48h at

R.T.

Heating rate : 90.0 /s

Holding time : 0,3,10 and 30min

Heating rate : 0.9 /s

1 _#120 2 _#800 3 _#1200 4 _#2400 5 MD-Dur _DP-DP-Spray (3µm) 6 MD-Chem OP-U

2 -Al Mg Si (Electron Probe Micro Analyzer EPMA )

JXA-8200M EPMA 2 -Al

Mg Si 2 2 Mg Si 2.2.6 2.2.7 Al Si Mg Fe 4 EPMA EPMA 2.2.6 2.2.7

Al

Si

Mg

Fe

Al

Si

Mg

Fe

CH-1:TAP CH-4:PETJ CH-2:TAP CH-5:LIFH

(kV)

20

(A)

3.0×10

-8

(µm)

0 or 2

Al

Si

Mg

Fe

Al

Si

Mg

Fe

CH-1:TAP CH-4:PETJ CH-2:TAP CH-5:LIFH

(kV)

20

(A)

2.5×10

-7

(µm)

1

0

(µm)

256×256

60×60

Si (Scanning

Electron Microscope SEM ) S-4500

2.2.8 SEM 2.2.8 SEM ! Si Scion Image Si 0.0443µm2_{(4 pixel)} ( / ) Si ! AutoSigma2000 ! 136 1.96N (200gf) 15s 2 [kg/mm2_]

HV =

2P sin68



d

2

× 1000

= 1.8544 ×

P

d

2

(kV)

15

Working Distance (mm)

15

(µA)

8 10

P [kg] d [mm] 2.5 (FUTURE-TECH FM-ARS 900) 0.049N(5gf) 15s -Al ! 2.4 AG50kNG 2.2.9 JIS ( 5mm 6mm ) 48 h 2 1.4 10-3_s-1 30 0.2% MoS2 2.2.9 ! 2.5 2.6 (0.2% ) AG50kNG 2.2.10 2.2.11 2.5 JIS7 ( 2mm 3mm 9.8mm) 48 h 2 8.5 10-4_s-1 ₃₀ 0.2% 2.6 ( 1mm 1mm 4mm) 48 h 3 2.1 10-3_s-1

Microstructure observation &

Electrical conductivity &

Hardness test

Compression test

Specimen

6mm

Φ5mm

Machining

Machining

30 0.2% 2.2.10 ( ) 2.2.11 ( )

2.3

2.3.1 ( 520 ) 2.3.1(a) K-type 0.5mm ( 5mm)

Microstructure observation & Electrical conductivity & Hardness test Tensile test Specimen 3mm 9.8mm 40mm 6mm t = 2mm R15mm Machining Machining 4mm 1mm t = 1mm Machining Specimen Machining

250 250 2.3.1(b) 560 2.3.2(a) 10mm 5 K-type 0.5mm L( 2.3.2(a) ) 2.3.2(b) (ch3) (Tchn-Tch3) (L=30mm ch4) L ch5 L=26mm 4 L=26mm 2.3.3 (a) 5 2mm 2.3.3(b) (ch3) (ch1 ch5) 5 ( ) 4 (L=26mm) (ch3 ) 9)

2.3.1

0

100

200

300

400

500

600

Thermocoupel

Radiation thermometer

Tem

per

at

u

re

,

T

/

Time ,

t

/ s

Stop heating

Start heating

5s

Extrapolated line

Measurable lower limit

of radiation thermometer

5mm L

(a)

Specimen Top view Heating coil

Measuring point using radiation thermometer

Side view

(b)

2.3.2 ch1 ch2 ch3 ch4 ch5 5mm L

(a)

Specimen Top view Heating coil

Measuring point using radiation thermometer Side view 10mm 10mm 10mm 10mm

-8

-6

-4

-2

0

2

4

6

L=24mm

L=26mm

L=28mm

L=30mm

T

chn

-T

ch3

/

ch1 ch2 ch3 ch4 ch5

(b)

2.3.3 2mm ch1…. 5

(a)

Heating coil Specimen

Measuring point using radiation thermometer 5mm Top view Side view L

-8

-6

-4

-2

0

2

4

6

No.1

No.2

No.3

No.4

No.5

T

chn

-T

ch3

/

ch1 ch2 ch3 ch4 ch5

(b)

2.4

40 /s (0.4 40 /s)

2.4.1

2.4.1 5 10 20 30 /min 4 10mg Al-Si 570 560 565 Al-Mg2Si-Si 11) _{450 570} 2.4.2 250 250 2.4.2 250 X Y Y 250 560 40.0 /s 250 Y 450 560 11s 14s 560 2.4.2(b) 2.4.3 -Al Si -Al

450 570 2.4.3 (h) 570 ( ) 2.4.2(b) 560 -Al Si Si 2.4.4 Si Si 2.4.4 Si 2.4.5 Si 2.4.6 0.2% 500 -Al Mg Si 570 500 500 ( ) G.P. 12) 520 Mg Si 0.2% 540 Si 570 2.4.3 (h) 570 560

2.4.1 2.4.2

540

560

580

600

620

640

Hea

t

fl

ow

,

H

Temperature , T /

10mW

5 /min

20 /min

10 /min

30 /min

Ts

570 5 569 10 570 20 569 30

0

100

200

300

400

500

600

570 560 540 520 500 450

Tem

per

at

u

re

, T

/

Time , t / s

40.0 /s Extrapolated line Measurable lower limit of radiation thermometer 5 s 400 450 500 550 600 1 s quench

(b)

(a)

2.4.5 Si 2.4.6

0

0.5

1.5

2.5

450

500

550

600

M

ea

n

a

rea

,

A

/μ

 m

2

Solution temperature , T /

3.0

2.0

1.0

3.0

2.5

2.0

1.5

1.0

0.5

0

M

ea

n

a

sp

ec

t

ra

ti

o

Mean area Mean aspect ratio

A

s-c

as

t

32.0

34.0

36.0

38.0

40.0

42.0

E

lec

tr

ic

al

c

on

du

ct

iv

it

y

,

(I

A

C

S

%)

30

40

50

60

70

80

90

60

80

100

120

140

160

180

450

500

550

600

Solution temperature , T /

V

ic

ker

s

h

ar

dn

es

s

, HV

0.

2%

pr

oof

st

res

s

,

0.2

/ M

Pa

A

s-c

as

t

Vickers hardness

0.2% proof stress

2.4.2

40.0 /s 560 2.4.7 40.0 /s 13s 560 ( 1 ) 560 4 2.4.8 Si Si Si 2.4.9 Si 3min 10min 0min 193% 264% 3min Si 3min Si Al Si Si 13) _{Al Si Si} Si Si Si Al Si Si Si Si Al Si 2.4.9 3min 2.4.10 0.2% 3min 3min Mg Si 3min 3min 3min α-Al 2.4.9 Si Si 3min (40.0 /s) ( 1 )

( 4 ) 2.4.7 2.4.8 Si

0

100

200

300

400

500

600

0

500

1000

1500

2000

Tem

per

at

u

re

,

T

/

Time , t / s

0 100 200 300 400 500 600 0 10 20 30 40 40.0℃/s Extrapolated line

Measurable lower limit of radiation thermometer 550 555 560 565 12 14 16 18 30 min 10 min 3 min 0 min Tf (℃) To (℃) 3 1 30 min 4 0 10 min 4 1 3 min 0 0 min To : Over heat Tf : Temperature fluctuation

(b)

(b)

(a)

2.4.9 Si 2.4.10

1.0

1.5

2.0

2.5

3.0

1.0

1.5

2.0

2.5

3.0

0

5

10

15

20

25

30

M

ea

n

a

rea

,

A

/

m

2

M

ea

n

a

sp

ec

t

ra

ti

o

Solution time ,

t

/ min

Mean area

Mean aspect ratio

0.5

0.5

0 0

A

s-c

as

t

32.0

34.0

36.0

38.0

40.0

42.0

E

lec

tr

ic

al

c

on

du

ct

iv

it

y

,

(I

A

C

S

)

30

40

50

60

70

80

90

60

80

100

120

140

160

180

0

5

10

15

20

25

30

Solution time , t / min

V

ic

ker

s

h

ar

dn

es

s

, HV

0.

2%

pr

oof

st

res

s

,

0.2

/ M

Pa

A

s-c

as

t

_{● Vickers hardness}

○ 0.2% proof stress

2.4.3

40.0 /s 560 3min 40.0 /s 4.0 /s 0.4 /s 3 2.4.11 560 2.4.12 Si Si 4.0 /s 0.4 /s Si 2.4.13 Si 40.0 /s 2.4.9 560 3min Si Si 40.0 /s Si ( 1.5µm2₎ 4.0 /s 0.4 /s 2.4.14 0.2% 0.4 /s 40.0 /s 5% 3% Si 40.0 /s Si ( 1.5µm2_{) 4.0 /s 168% 0.4 /s 149%}

2.4.11 2.4.12 Si 560 25 s 5 40.0 /s 4.0 /s 0.4 /s 0 100 200 300 400 500 600 0 500 1000 1500 2000 Tem per at u re ,

T

/ Time ,

t

/ s 40.0 /s Extrapolated line

Measurable lower limit of radiation thermometer 4.0 /s

0.4 /s

(a)

2.4.13 Si 2.4.14

1.0

1.5

2.0

2.5

3.0

1.0

1.5

2.0

2.5

3.0

M

ea

n

a

rea

,

A

/

m

2

M

ea

n

a

sp

ec

t

ra

ti

o

Heating rate ,

V

/ (

・s

-1

)

0.5

0.5

0

0

A

s-c

as

t

Mean area

Mean aspect ratio

1

10

10

2

32.0

34.0

36.0

38.0

40.0

42.0

E

lec

tr

ic

al

c

on

du

ct

iv

it

y

,

(I

A

C

S

)

30

40

50

60

70

80

90

60

80

100

120

140

160

180

V

ic

ker

s

h

ar

dn

es

s

,

HV

0.

2%

pr

oof

st

res

s

,

0.2

/ M

Pa

A

s-c

as

t

1

10

10

2

Heating rate ,

V

/ (

・s

-1

)

● Vickers hardness

○ 0.2% proof stress

2.5

Mg Si Si

2.5.1

2.5.1.1 Mg Si EPMA Mg Si 2.5.1 2 Al Fe Mg Si 4 Al -Al -Al Si Si Si Si Mg Fe Mg Fe 2.5.2 2.5.2(a) 2 Al Fe Mg Si 4 Al-Fe-Mg-Si 2.5.2(b) 2 4 2.5.2(a) Al-Fe-Mg-Si 2.5.2(c) 2 Mg Si Mg2Si 2 Mg 2 Fe Mg2Si 3 2.5.3 (Mg Fe ) (IH:0min) Mg Fe 3min Fe Mg (EF) Mg (560 ) 25 Mg

3 2.5.4 Fe Mg2Si 0min 2 Fe Mg2Si 3min Fe Fe Fe ( 2.5.3) Mg Al-Fe-Si 560 ( 30min) Fe Fe Fe EPMA Fe 30min Fe 10 2.5.1 Fe Al Mg Si Fe Fe 30min Fe Mg Al-Fe-Si Fe 14) 16) _AC4CH A356 Fe 17)

α-AlFeSi(Al8Fe2Si) -AlFeSi (Al5FeSi)

Mg -AlFeMgSi (Al8FeMg3Si618),19) Al9FeMg3Si520),21) ) 22),23) 24) Fe 2.5.1 Closset 18) _Gustafsson 19) (Al8FeMg3Si6) Fe Fe EPMA Fe Closset 18) _{Fe Mg (0.16%Fe-0.45%Mg)} Mg -AlFeSi 22),23) _Fe

Mg 2

Fe 3min Mg

( 2.5.3) 30min Fe

Mg ( 2.5.1) 3min -AlFeSi

2.5.2 EPMA (a) Al-Fe-Mg-Si

( ) (b) Al-Fe-Mg-Si ( )

2.5.3 EPMA

2.5.1 (mass%) 2.5.1.2 α-Al Mg Si Mg2Si Mg 3min Mg α-Al α-Al Mg EPMA Si 2.5.5 α-Al ( 20 m 30 m) 2 3 2 m α-Al Mg Si 3 α-Al 2.5.5 ( ) Mg

0min 0min 3min

3min 0.37% Mg Mg α-Al Si 0min 3min Mg Si 1.50% Al-Si 2 1.65%(577 )25) ₅₆₀ α-Al Mg Si 560 Al Mg Si x[m] 26)

Intermetallic compound Al Fe Mg Si Reference

Chinese script-like 72 1 17 10

Present work

Plate-like 65 2 20 13

Plate-like

(Solution treated for 30 min) 89 3 0 8

-Al8FeMg3Si6 52 10 13 28 B.Closset

18)

(2.1) (2.2) D [m2_{/s] t [s] D0 [m}2_{/s] Q [kJ/mol] R} (8.3145[J mol-1 _K-1_{]) T [K] Mg Si D0 1.24} 10-4 _{3.5 10}-5 _{Q 131 124} 27) _{α-Al Mg} Si 3min Mg Si x Mg Si 11.4 m 10.2 m Mg Mg 102µm×136µm 102µm×136µm Mg 2.5.1 5 66µm 3min Mg 11.4µm Mg ( 66µm) 17% Mg 3min -Al Mg 2.5.5 3min -Al Mg Mg -Al Mg -Al Mg Mg Si -Al -Al Mg 28) _-Al Mg 2.5.6 ( 2.5.6 (a)) Mg -Al ( 2.5.6 (b) 3min ) Mg Mg -Al ( 2.5.6 (c) 3min ) -AlFeSi Mg -Al Mg

x = Dt

€

D = D

0

exp(−

Q

RT

)

20 m -Al Mg 3min Si Si 2.5.5 -Al Mg Si Mg2Si Mg2Si Mg Si -Al 2.5.5 α-Al Mg Si

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

1.5

2.0

2.5

0

5

10 15 20 25 30

C

on

cen

tr

at

ion

of

M

g

(m

as

s%)

Solution time ,

t

/ min

C

on

cen

tr

at

ion

of

S

i (m

as

s%)

A

s-c

as

t

EF

0.5

Mg

Si

Primary α-aluminum phase

Eutectic

region

Analysis

points

2.5.6 Mg (a) (b) (c) 2.5.1.3 -Al Mg -AlFeSi Mg ( 2.2.7 a.b) -AlFeSi ( a,b c,d ) 2.5.7 2.5.2 c,d a,b 3.2 1.8 2.5.8 a,b 1,3,5 7min c,d Mg (a) (b)

Primary α-aluminum phase Eutectic Si particle π-phase(Chinese script-like) (c) β-AlFeSi(not containing Mg) π-phase (Plate-like)

-Al Mg 1min Mg Mg Fe ( -AlFeSi) 3min Mg α-Al Mg 5min Mg α-Al Mg c,d Mg -AlFeSi c,d 2.5.9 c,d Mg 3min 3.2 1.8 a,b 7min Mg 5min 2.5.8 7min Mg Fe Si Mg2Si 560 Al-Si-Mg2Si 3 559 11) Mg2Si 560 2.5.2 Specimen c,d a,b DAS (µm) 21.7 33.9 Mean area (µm2₎ - phase (Chinese script-like) 26.0 82.4 - phase (Plate-like) 16.4 25.6 Eutectic Si particle 0.9 3.6

2.5.8 EPMA

2.5.9

Solution time (min)

0 3 As-cast 1 5 7 Specimen Intermetallic compounds -phase (Chinese script-like) -phase (Plate-like) Mg2Si c,d exist (containing Mg) exist exist transformation (not containing Mg) a,b c,d a,b c,d a,b

2.5.1.4 Si 2.5.10 ( c,d) Si Si ( / ) 2.5.11 1 5 0min 3min 2.5.5 3min Si Si 3min Si 3min 2.5.10

2.5.11 Si

2.5.2

2.5.2.1 0.2% -Al 2.5.12 -Al 10 2 8 8 -Al 0.2% 0min 3min 21% 0.2% 23% 3min

0

2

4

6

8

10

12

1.0

1.5

2.0

2.5

3.0

0

5 10 15 20 25 30

M

ea

n

a

rea

,

A

/

m

2

M

ea

n

in

ter

pa

rt

ic

le

di

st

an

ce

, d

/

 m

M

ea

n

a

sp

ec

t

ra

ti

o

Solution time , t / min

A

s-c

as

t

EF

0.5

0

Mean area

Mean aspect ratio

3min 3min Si 560 3min ( EF 535 480min) 2.5.12

60

65

70

75

80

85

V

ic

ker

s

h

ar

dn

es

s

,

HV

100

110

120

130

140

150

160

0

10

20

30

40

50

60

0

5 10 15 20 25 30

0.

2%

pr

oof

st

res

s

,

σ

0.2

/

M

Pa

Solution time,

t

/ min

Fr

ac

tu

re

el

on

ga

ti

on

,

ε

(%)

Fracture elongation

A

s-c

as

t

EF

0.2% proof stress

2.5.2.2 Mg Si 2.5.12 -Al 0.2% Mg Si 2.5.5 -Al Mg Si 0.2% ( ) 2.5.13 3min α-Al Mg Si 3min -Al Mg Si 29) _Cottrell30) _Friedel31) Δσ (2.3) ( 0.34732)_{) M (3.06}29)_{) (} 26.5[GPa]32)_{) [%] c [at.%] (1) c} 3min -Al Mg Si ( ) (Mg ΔσMg Si ΔσSi) 2.5.5 3min -Al Mg Si 0.20[at.%] 0.16[at.%] Al Mg Si 0.96[%] -0.6[%]33) _{ΔσMg ΔσSi}

12[MPa] 5[MPa] 17[MPa] 2.5.12

3min 0.2% 27[MPa] (1) 60% 2.5.5 3min Mg Si Mg Si ( ) 29) 3min -Al Mg Si Al

Δσ =

3

3/4

2

1+ν

1−ν

#

$

%

&

'

(

3/2

Mµ ε

3/2

c

Al (1) Al-Mg-Si Si 34) 35) _{Mg2Si Al-7%Si-Mg Si} 48 ( 5min) 3,000min(50 ) 3% ( 2.8 ) 36) -Al Mg Si ( ) α-Al Mg Si (n ) 2.5.14 n n 1% 0min n 3min n n 37) 38) Al-Mg 2 Mg 39) _3min -Al Mg Si 2.5.12 -Al Mg Si Mg Si

2.5.13 α-Al Mg Si 2.5.14 n

120

125

130

135

140

145

150

155

0.1

0.2

0.3

0.4

0.5

0.6

1.1

1.2

1.3

1.4

1.5

1.6

Mg

Si

0.

2%

pr

oof

st

res

s

,

0.2

/ M

Pa

Concentration of Mg ,

CMg

(mass%)

Concentration of Si ,

CSi

(mass%)

As-cast

IH:0min

IH:3 to 30min & EF

0.10

0.15

0.20

0.25

0

5

10

15

20

25

30

35

n value

As-cast

IH:0min

IH:3min

IH:10min

IH:30min

EF

True strain ,

ε

t

(%)

0.05

2.5.2.3 Si DAS Fe Si 40) 2.68[Mg/m3_{] AC4CH} 41) DAS Fe (0.12%) Fe Fe 42) _Si Si Si 43) _3min Si 3min Mg Si 3min Si -Al Si SEM 2.5.15 3min Si Si 40) _X CT 44),45) 46) _Si Si Si Si 2.5.16

Si ( 2.5.16 (a)) ( 2.5.16 (b)) Si 45)_{( 2.5.16 (c)) Si} 24) _Si ( 2.5.16 (d)) 2.5.16 3 1 5 6 Si 5 6 Si Si Si Si 1 5 47) _{2.5.15 SEM} (2.4) D [µm] L [µm] nL Si 2.5.17 (D) Si ( ) (2) D 47) Hensler 48) _1.62 Dc(Dc=1.62D) 2.5.17 (D) (Dc) 3min Si 3min Si 3min Si 3min 2.5.11 Si Si 43) Si

D =

L

n

_L

Si 2.5.15 2.5.16 (a) (b) (c) Si (d)

Loading direction

Loading direction

(b)

(d)

Dimple

Eutectic Si particle

(a)

α-aluminum phase

Hydrogen micropore

(c)

Damage

2.5.17 Si

2.6

Si

2.1.2 Si Si Si 10) _Si Si SEM

2.6.1

Si

2

4

6

8

10

12

2

4

6

8

10

12

D

Dc

Mean interparticle distance between

eutectic Si particles ,

d

/  m

M

ea

n

d

ia

m

et

er

of

di

m

pl

es

,

D

and

Dc

/ μ

m

Solution time : 3min

Solution time :10min

90.0 /s( ) 0.9 /s 2 560 0,3,10 30min 4 Si 2.6.1 2.6.2 90.0 /s ( 2.6.1) 6s 560 7 20s (560 ) 1 4 20s 560 40.0 /s ( 2.4.7 ) 40.0 /s Mg2Si ( 0min) 90.0 /s 40.0 /s Mg2Si Mg2Si Mg2Si 0.9 /s ( 2.6.2) 560 600s 4 (560 1 3 ) 2.6.1 (90.0 /s)

0

100

200

300

400

500

600

0

500

1000

1500

2000

Tem

per

at

u

re

,

T

/

time ,

t

/ s

530

535

540

545

550

555

560

565

570

5

10

15

20

25

30

Region of temperature depression

To

30min 10min 3min 0min To ( ) 7 5 3 2

2.6.2 (0.9 /s) 2.6.3 0 3 30min 90.0 /s 0min Si 3min 0min Si 30min 0.9 /s 0min Si 0min 0.9 /s 90.0 /s Si 30min Si Si ( / ) 2.6.4 2.5.1.4 1 5 90.0 /s 0min 60% 3min 10min 30% 30min 84%

0

100

200

300

400

500

600

0

500

1000

1500

2000

2500

Tem

per

at

u

re

,

T

/

time ,

t

/ s

530

535

540

545

550

555

560

565

570

590

595

600

605

610

Tf

30min 10min 3min 0min Tf ( ) 4 4 4

0.9 /s 0min 90.0 /s

90.0 /s 14%

3min

13% 10min 49% 30min 86% 30min

90.0 /s 90.0 /s 10min 10min 0.9 /s 30min 30min 90.0 /s Si Chaudhury 10) _{90.0 /s} 0min 0min Si ( ) 0.9 /s 30min 90.0 /s Si Si SEM Si (HCl 15ml HF 10ml 90ml) 55 (HNO3 25ml 75ml) 4 Al SEM 2.6.5 0 3 30min Al Si Si 90.0 /s 0min Si 2 Si 2 Si 90.0 /s 3min Si 1 2 Si 90.0 /s 30min Si 0.9 /s 0min Si 90.0

/s 3min 1 2 0.9 /s 3min 0min 0.9 /s 30min Si 30min Si Si ( ) SEM Si (90.0 /s) 0min Si 0min Si SEM 90.0 /s 0min Si 2 2 Chaudhury 10) _{Al Si} Si Si Si 90.0 /s 440 560 ( ) Si SEM 90.0 /s 2.6.6 Si Si 2.6.7 Si 500 2.6.8 Si SEM Si 1 2 Si 560 2 1 ( 2.6.8(a)) 2.6.9 500 Si Si Si 2 Si 2 Si Si Si

Si Al ( ) Al Si Si Si 3 ( ) 49) _Al Si 2.5.1.2 (2.2) 560 Al Si D 5.8 10-13 _[m2_{/s] ( D0 3.5} 10-5 _[m2_{/s] Q 124 [kJ/mol] R 8.3145 [J mol}-1 _K-1_] T 833 [K] (560 ) ) Si Si Si Si Bracht 50) 28_{Si Si} 855 Si D 2 5 10-15_[m2_{/s] 855} Si Bracht 50) 560 D (0.6 1.0) 10-22_[m2_/s] Si Si Al Si Si (90.0 /s) Si Al ( ) Si 2 Si 0.9 /s Si 2 Si Si Al Si 2 Si Si Si (90.0 /s) ( 0min) Si Si Si 2.6.10 Si 1 2

(90.0 /s) Si Al Si ( ) 2 0.9 /s 2 Al Si Si Al Si Si Si

2.6.3 Si ( )

2.6.4 Si

1.0

2.0

3.0

4.0

5.0

1.5

2.0

2.5

3.0

3.5

4.0

0

5

10

15

20

25

30

Solution time , t / min

M

ea

n

a

rea

,

A

/

m

2

M

ea

n

a

sp

ec

t

ra

ti

o

A

s-c

as

t

0

M

ea

n

in

ter

pa

rt

ic

le

di

st

an

ce

bet

w

een

eu

tec

ti

c

S

i p

ar

ti

cl

es

, l

/

m

Mean area

Mean interparticle distance

Mean aspect ratio

90.0 /s

0.9 /s

2.6.7 (90.0 /s) Si

1.0

1.5

2.0

2.5

3.0

3.5

1.0

1.5

2.0

2.5

3.0

450

500

550

600

M

ea

n

a

rea

,

A

m

2

M

ea

n

a

sp

ec

t

ra

ti

o

Solution temp. , T /

A

s-c

as

t

0.5

0

0.5

Mean area

2.6.8 (90.0 /s) Si (SEM )

2.6.10 Si

0.9 /s_0min 0.9 /s_3min 0.9 /s_30min

90.0 /s_0min

Eutectic Si particles

As-cast 90.0 /s_3min 90.0 /s_30min

Eutectic Si particles / Al matrix interface

Al matrix

Eutectic Si particles

Diffusion of Si atoms

D iffu si on s peed Hi gh S low Staying time at high temp.

+ +

E u tec ti c S i p ar ti cl es C oa rs en in g R efi n em en t

2.6.2

2.6.11 2.6.12

0.2% 0.2%

10min 10min 10min 0.2%

2.5.1 Al (Mg Si) 0.2% 6% 0.2% 2.6.13 3min 3min (90.0 /s) 0min 30min 90.0 /s 0.9 /s 30min 2.6.13 2.6.11 0.2% 51) _Al-Si Si Si Si 2.6.13 Si 2.6.11 0.2% ( 2.6.12) 90.0 /s 0.9 /s 6%(3min) 37%(10min) 10% SEM 2.6.14 Al 52) 58) _2.6.15

2.6.12 Si 0 3 30min 2.6.16 2.6.17 2.6.4 ( 2.5.2.3 ) 2.6.17 2.5.2.3 90.0 /s 0min 28% 5% 2.6.18 90.0 /s 0min Si 2 3min Al Si 90.0 /s 0.9 /s 2.6.11 90.0 /s 90.0 /s

2.6.11 0.2% 2.6.12

100

110

120

130

140

150

160

0

5

10

15

20

25

30

0.

2%

pr

oof

st

res

s

, σ

0.2

/M

Pa

A

s-c

as

t

Solution time , t / min

90.0 /s

0.9 /s

0

5

10

15

20

25

0

5

10

15

20

25

30

A

s-c

as

t

Solution time ,

t

/ min

Fr

ac

tu

re

el

on

ga

ti

on

,

ε

(%)

90.0 /s

0.9 /s

2.6.13

2.6.14 SEM (a) (b) 90.0 /s 0min (c) (d)

0.9 /s 0min

33.0

34.0

35.0

36.0

37.0

38.0

0

5

10

15

20

25

30

90.0 /s

0.9 /s

Solution time ,

t

/ min

E

lec

tr

ic

al

c

on

du

ct

iv

it

y,

ρ

(I

A

C

S

%)

A

s-c

as

t

2.6.15

0

5

10

15

20

25

0

5

10

15

20

25

30

90.0 /s_ 0min

90.0 /s_ 3min

90.0 /s_10min

90.0 /s_30min

0.9 /s_ 0min

0.9 /s_ 3min

0.9 /s_10min

0.9 /s_30min

As-cast

Fr

ac

tu

re

el

on

ga

ti

on

,

(%)

Area ratio of defects

in fracture surface ,

f

(%)

2.6.17

2.0

2.5

3.0

3.5

4.0

4.5

5.0

2.0

2.5

3.0

3.5

4.0

4.5

5.0

As-cast

90.0 /s

0.9 /s

M

ea

n

d

ia

m

et

er

of

di

m

pl

es

,

D

/

m

Mean interparticle distance between

eutectic Si particles ,

d

/ μm

0min

3min

10min

2.6.18 90.0 /s_0min (a) (b) (c) Si (d)

2.7

FSP FSP ( ) 1. 2.3 (L=26mm) 4 4 2. 2.4 (40.0 /s) Dimple Eutectic Si particle Hydrogen micropore Damage

A

s-c

as

t

90.0

/s

_0

m

in

(a)

(b)

(c)

(d)

Loa

di

n

g

di

rec

ti

on

40.0 /s Si 560 ( : 40.0 /s) Si 3min Si Si Si 40.0 /s ( 1.5µm2_{) 4.0 /s 168% 0.4 /s 149%} 3. 2.5 (40 /s) (560 ) 0min 30min) Mg Si Si Mg2Si Mg Mg2Si 560 3min Mg -AlFeSi Mg Mg Mg Mg 3min -AlFeSi 40.0 /s 560 3min -Al 0.2% 21% 23% 3min 0.2% (535 -480min) 3min 30min 3min -Al Mg Si 0.2%

-Al Mg Si Si 3min Si 40 /s 560 3min (535 -480min) FSP 560 -3min 4. 2.6 Si SEM 90.0 /s 560 ( 0min) Si SEM Si 2 560 Si 0.9 /s 560 Si 30min Si ( ) Si Si 10min 10min (90.0 /s) 6% Si 90.0 /s 0.9 /s 10% SEM Al

2.8

1

560 30min

10000min 2.8.1 2

No.1 No.2 0.8 IACS%

2.2.1 c, d No.2 3000min 3% Al 36) 3000min 2880min(48h) 2.8.1

34.0

35.0

36.0

37.0

38.0

39.0

40.0

10

10

2

10

3

10

4

No.1

No.2

time , t / min

E

lec

tr

ic

al

c

on

du

ct

iv

it

y,

(I

A

C

S

%)

A

s-c

as

t

1) D.L.Zhang L.H.Zheng D.H.StJohn J.Light Metals 2 (2002) pp.27-36 2) S.K.Chaudhury L.Wang D.Apelian AFS Transactions (2004) pp.289-304

3) Vol.55 No.4 (2005) pp.159-163.

4) Y.Harada S.Tamura S.Kumai Mater. Trans. Vol.52 No.5 (2011) pp.848-855.

5) (

) No.58(2012) pp.57-61.

6) Vol.40 No.8 (1990) pp.533-537.

7) J.C.Choi H.J.Park B.M.Kim J. Mater. Process. Technol. Vol.87 (1999) pp.46-52. 8) H.K.Jung C.G.Kang J. Mater. Process. Technol. Vol.104 (2000) pp.244-253. 9)

(2012).

10) S.K.Chaudhury D.Apelian Metal. Mater. Trans. A Vol.37A (2006) pp.763-778. 11) ASM Metals Handbook 8th ed. (1973) ASM pp.360.

12) Vol.23 No.8 (1973) pp.354-359.

13) : Vol.20 No.5 (1970) pp.247-255.

14) Vol.19 (1955) pp.197-201

15) S.G.Shabestari : Mater. Sci. Eng. A 383 (2004) pp.289-298.

16) Vol.83 No.1 (2011) pp.47-57

17) Vol.56 No.1 (2006) pp.21-27

18) B.Closset J.E.Gruzleski : Metall. Trans. A Vol.13A No.6 (1982) pp.945-951

19) G.Gustafsson, T.Thorvaldsson, G.L.Dunlop : Metall. Trans. A Vol.17A No.1 (1986) pp.45-52 20) Q.G.Wang, C.J.Davidson : J. Mater. Sci. Vol.36 (2001) pp.739-750

21) R.Krendelsberger, P.Rogl, A.Leithe-Jasper, C.J.Simensen : J. Alloys and Compounds Vol.264 (1998) pp.236-239

22) A.M.Kliauga, E.A.Vieira, M.Ferrante : Mater. Sci. Eng. A Vol.480 (2008) pp.5-16

23) J.A.Taylor, D.H.St John, J.Barresi, M.J.Couper : Mater. Sci. Forum Vols.331-337 (2000) pp.277-282

24) K.Lee, Y.N.Kwon, S.Lee : J. Alloys and Compounds Vol.461 (2008) pp.532-541

25) 40 ( ) (1991) pp.231.

27) 40 ( ) (1991) pp.4

28) ( ) (2005) 299

29) Vo.60 No.9 (2010) pp.458-466

30) A.H.Cottrell Strength of Solids (Phys. Soc. London) (1948) pp.30-36. 31) J.Friedel Dislocations (Pregamon Press New York) (1964) pp.205

32) J.P.Hirth, J.Lothe : Theory of Dislocations second edition (Wiley New York) (1982) pp.837 33) Vol.60 No.8 (2010) pp.411-418 34) Vol. 51 No.4 (2001) pp.215-221 35) Vol.28 No.11 (1978) pp.531-540 36) Vol.28 No.11 (1978) pp.553-557 37) Vol.45 No.4 (1995) pp.193-197 38) Vol.31 No.5 (1981) pp.359-368 39) Vol.41 No.2 (1991) pp.119-125 40) Vol.41 No.6 (1991) pp.398-405 41) 40 ( ) (1991) pp.520 42) Vol.64 No.8 (1992) pp.531-536

43) Mahmoud Fouad HAFIZ Vol.43 No.9 (1993)

pp.472-477

44) Vol.58 No.2 (2008) pp.58-64

45) H.Toda H.Ooga K.Uesugi M.Kobayashi Mater. Trans. Vol.50 No.9 (2009) pp.2285-2290

46) Vol.59 No.1 (2008)

pp.30-34

47) Vol.44 No.1 (1994) pp.48-56 48) J.H.Hensler J. Ins. Metals 96 (1968) 190

49) ( ) (2005) pp.299

50) H.Bracht E.E.Haller R.C.Phelps Phys. Rev. Lett. Vol.81 No.2 (1998) pp.393-396.

51) Vol.41 No.8 (1991) pp.510-514

52) C.H.Caceres B.I.Sellong Mater. Sci. Eng. A220 (1996) pp.109-116.

53) Vol.70 No.4 (1998) pp.254-259.

54) A.M.Gokhale G.R.Patel Mater. Chara. Vol.54 (2005) pp.13-20.

55) J.A.Francis G.M.Delphine Cantin Mater. Sci. Eng. A407 (2005) pp.322-329. 56) A.M.Gokhale G.R.Patel Scr. Mater. Vol.52 (2005) pp.237-241.

57) C.D.Lee Mater. Sci. Eng. A464 (2007) pp.249-254.

3

Si

3.1

3.1.1

FSP

Si

1 AC4CH ECAP ARB

-Al Si Si Si Si Si Si ECAP Si Si

3.2

! AC4CH (JIS ) Ar Sr Si ( ) 3.2.1 3.2.1 15mm 40mm 5mm ECAP

3.2.1 AC4CH (mass%) 3.2.1 ! 3.2.2 ECAP ECAP 550 2 ( ) 1) ECAP Si ECAP ECAP 350 30min

Si

Fe

Cu

Mn

Mg

Zn

Ti Sr(ppm) Al

Sample 7.4

0.11 <0.01 0.01 0.34 <0.01 0.12

107

bal.

8mm

Ingot

190mm

22mm

40mm

15mm

5mm

3.2.2 ! ECAP ECAP Si ECAP 3.2.3 5mm 15mm 120 16 ECAP Route A 2) _ECAP MoS2 2 4 8 4 ECAP 2 ECAP N 3)

ε

N

=

N

3

2 cot

φ

2

+

ψ

2

!

"

#

$

%

& +ψ cosec

φ

2

+

ψ

2

!

"

#

$

%

&

'

(

)

*

+

,

(3.1) N ECAP ECAP 3.2.2

550

2h

350 -30min

Tem

p.

time

ECAP

2,4,6 and

8pass

•  Tensile test

•  Microstructure observation

3.2.3 ECAP 3.2.2 ECAP ! ECAP Si ( ) USB (L-830) (Scion Image) Si SEM( S-4500) Si

Φ = 120°

Channel

(Section size :

5mm×15mm)

ECAP

die

ψ = 16°

Specimen

Rou

te A

Number of ECAP Pass

N

2 4 6 8 Equivalent plastic strain

ε

N 1.28 2.56 3.84 5.12

! Si AG50kNG 3.2.4 ECAP 10mm 5mm 2 ( 1mm 4mm) 4 2 ECAP 2.1 10-3_s-1 0.2% 3.2.4

12mm

23mm

40mm

7.5mm

15mm

5mm

10mm

5mm

4mm

1mm

1mm

Tensile specimen

Tensile direction

Extrusion direction

3.3

3.3.1 ECAP

ECAP 3.3.1 5mm 15mm X 5mm 40mm Y 15mm 40mm Z X Y Z -Al ECAP 2 X Z Y Z 2 -Al Z ECAP X 2 Y ECAP Si Z Z ECAP ECAP 2),4) _Wu 4) _3.3.2 ECAP (Route A) Y ECAP ECAP ECAP ( ) 3.3.3 ECAP Y ECAP Si Si ( ) 6 ECAP Si 6 Si 3.3.1 ECAP Si Wu 4) 6 Y Si Furukawa 2) _ECAP ( Furukawa 2) ) Furukawa 2)

Route A ECAP ECAP X Z

Y Wu 4)

ECAP Z

Furukawa 2)

( 3.3.1 ) 3.3.1 ECAP

3.3.1 ECAP (a) ECAP (b) 2 (c)

3.3.2 Wu 4) _ECAP

ECAP die

Channel

Specimen

Shear

plane

Shear

directions

E

xt

ru

si

on

d

ir

ec

ti

on

E

xt

ru

si

on

d

ir

ec

ti

on

θ

3.3.3 ECAP Y (a) ECAP (b)

2 (c) 4 (d) 6 (e) 8

3.3.1 ECAP Y

Number of ECAP Pass

N

0

1

2

3

4

5

6

7

8

Inclination

angle

θ

(deg.)

Present works

25

14

9

10

3.3.2

Si

3.3.1 Si 2 5) _f

f =

1−V

V

N

_L (3.2) VV 2 NL 2 2 r

r =

3V

V

4N

_L (3.3) f (3.2) (3.3)

f =

4r(1−V

V

)

3V

_V (3.4)

δ =

2

3

r

m

π

V

_V

!

"

#

$

%

&

1/2

− 2

(

)

*

+*

,

-*

.*

(3.5) rm 2 2 2 2 Si Si -Al Si Si Si 3.3.4 ( 20 m 20 m )

Si ( 3.3.4 Si Si ) Si -Al Si Si Si Si ( Si ) ( Si ) (Coefficient of Variation CV ) CV Si CV ( Si Si ) Si CV Si Si Si 102 m 136 m 102 m 136 m Si ( -Al Si ECAP ) ECAP 8 X 10 10 m 10 m 20 m 20 m 30 m 30 m 40 m 40 m 4 Si 3.3.5 20 m 20 m Si 20 m 20 m -Al Si ECAP 8 20 m 20 m Si Si Si

20 m 20 m ECAP Si ECAP 2 4 8 Si 3.3.6 3.3.7 (Y 3.3.3 ) X ( 3.3.6) -Al ECAP 2 -Al Si Y ( 3.3.3) -Al ECAP 2 -Al Si ECAP Si (ECAP Si 1 ) Z ( 3.3.7) ECAP Si 20 m 20 m Si 3.3.8 3.3.10 3.3.8 3.3.10 10 X ( 3.3.8) Si ECAP Si Si Y ( 3.3.9) X ECAP Z ( 3.3.10) ECAP ECAP Si ( ) ( ) (CV ) 3.3.11 X ECAP 2 CV 40% Y ECAP CV 8 ECAP CV 56% Z ECAP CV 3.3.3 3.3.6 3.3.7 Si 3.3.11 CV CV Si Si

3.3.4 Si

Fr

eq

u

en

cy

Number of eutectic Si particles

in a grid

As-start

ECAP processed

Count of number of eutectic Si particles in a grid

Fr

eq

u

en

cy

Number of eutectic Si particles

in a grid

Calculation of coefficient of variation (

CV

)

CV =

σ

µ

σ : standard deviation

µ : arithmetic mean

136 µm

102 µm

Grid size : 20µm×20µm

3.3.5 Si 0 100 200 300 400 500 600 0 2 4 6 8 10 0 10 20 30 40 50 60 0 4 8 12 16 20 24 0 5 10 15 20 25 30 0 10 20 30 40 50 0 5 10 15 0 10 20 30 40 50 60 70 80 Number of eutectic Si particles in a grid , N 0 100 200 300 400 500 600 0 2 4 6 8 10 Fr eq u en cy 0 10 20 30 40 50 60 0 4 8 12 16 20 24 Fr eq u en cy 0 5 10 15 20 25 30 0 10 20 30 40 50 Fr eq u en cy 0 5 10 15 0 10 20 30 40 50 60 70 80 Fr eq u en cy Number of eutectic Si particles in a grid , N

As-start

ECAP _ 8 pass

10µm

×

10µm

20µm

×

20µm

30µm

×

30µm

40µm

×

40µm

G

ri

d

si

ze

3.3.6 ECAP X (a) ECAP (b) 2

3.3.7 ECAP Z (a) ECAP (b) 2

3.3.8 X Si (a) ECAP (b) 2 (c) 4 (d) 6 (e) 8

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

0

10

20

30

40

50

60

0

5

10

15

20

25

30

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

Number of eutectic Si particles

in a grid ,

N

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Number of eutectic Si particles

in a grid ,

N

Specimen

(a)

(b)

(c)

3.3.9 Y Si (a) ECAP (b) 2 (c) 4 (d) 6 (e) 8

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Number of eutectic Si particles

in a grid ,

N

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

Number of eutectic Si particles

in a grid ,

N

0

10

20

30

40

50

60

0

5

10

15

20

25

30

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

Specimen

(a)

(b)

(c)

(d)

(e)

3.3.10 Z Si (a) ECAP (b) 2 (c) 4 (d) 6 (e) 8

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Number of eutectic Si particles

in a grid ,

N

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

Number of eutectic Si particles

in a grid ,

N

0

10

20

30

40

50

60

0

5

10

15

20

25

30

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

0

10

20

30

40

50

60

0

5

10

15

20

25

30

Fr

eq

u

en

cy

Specimen

(a)

(b)

(c)

(d)

(e)

3.3.11 ECAP CV

3.3.3

Si

Si (CV ) ECAP 0.2% 3.3.12 ECAP 6 ECAP 78MPa ECAP 125MPa ECAP ECAP ECAP (0.2% ) ECAP 3.3.13 1.96N (200gf) 15s ECAP 2 84%

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

0

2

4

6

8

C

oeffi

ci

en

t

of

va

ri

at

ion

,

CV

Number of ECAP processed pass

X plane

Y plane

Z plane

1.0

A

s-s

ta

rt

6 2 350 30min ECAP ECAP ECAP ECAP Si ECAP 3.3.14 ECAP ECAP 8 49% 64% 54% 6 3.3.12 3.3.15 ECAP 3.3.16 Si Si Si 3.3.12 ECAP 0.2%

60

70

80

90

100

110

120

130

140

0

2

4

6

8

0.

2%

pr

oof

st

res

s

,

0.2

/ M

Pa

Ten

si

le

st

ren

gt

h

,

b

/ M

Pa

A

s-s

ta

rt

0.2% proof stress

Tensile strength

3.3.13 3.3.14 ECAP

30

40

50

60

70

80

90

0

2

4

6

8

Number of ECAP processed pass

V

ic

ker

s

h

ar

dn

es

s

,

HV

Before annealing

After annealing

A

s-s

ta

rt

0

10

20

30

40

50

0

2

4

6

8

Fr

ac

tu

re

el

on

ga

ti

on

,

(%)

U

n

ifor

m

el

on

ga

ti

on

,

u

(%)

Loc

al

el

on

ga

ti

on

,

l

(%)

Fracture elongation

Uniform elongation

Local elongation

A

s-s

ta

rt

3.3.15 (a) ECAP (b) 2 (c) 4

3.3.16 Si (ECAP 8 ) Si 3.3.17 3.3.19 ECAP CV ( ) X ( 3.3.17) ECAP X X Si ECAP CV ( Si ) ECAP CV CV Y ( 3.3.18) ECAP CV CV CV CV Z ( 3.3.19) ECAP CV CV X Si Y Si 3.3.20 (Y Z ) Y

Z 3 Si 3.3.21 ECAP CV ((CVX+CVY+CVZ)/3) CV CV Si Si CV Si Si 3.3.17 X CV

60

80

100

120

140

160

0

10

20

30

40

50

0

0.2

0.4

0.6

0.8

1.0

E

lon

ga

ti

on

,

(%)

0.

2%

pr

oof

st

res

s

,

0.2

/

M

Pa

Ten

si

le

st

ren

gt

h

,

b

/

M

Pa

Coefficient of variation of X plane , CV

X

Fracture elongation

Uniform elongation

Local elongation

Tensile strength

0.2% proof stress

A

s-s

ta

rt

ECAP processed

3.3.18 Y CV 3.3.19 Z CV

60

80

100

120

140

160

0

10

20

30

40

50

0

0.2

0.4

0.6

0.8

1.0

Fracture elongation

Uniform elongation

Local elongation

Tensile strength

0.2% proof stress

A

s-s

ta

rt

ECAP processed

E

lon

ga

ti

on

,

(%)

0.

2%

pr

oof

st

res

s

,

0.2

/

M

Pa

Ten

si

le

st

ren

gt

h

,

b

/

M

Pa

Coefficient of variation of Y plane , CV

Y

60

80

100

120

140

160

0

10

20

30

40

50

0

0.2

0.4

0.6

0.8

1.0

Fracture elongation

Uniform elongation

Local elongation

Tensile strength

0.2% proof stress

E

lon

ga

ti

on

,

(%)

0.

2%

pr

oof

st

res

s

,

0.2

/

M

Pa

Ten

si

le

st

ren

gt

h

,

b

/

M

Pa

Coefficient of variation of Z plane , CV

Z

As-start