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Page 1: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 16

Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio andTemperature Effect on the Microstructure and Mechanical Properties

Peres M M1Fogagnolo JB

1 AH

1 Audebert F

2 Saporiti F

2 Jorge Jr AM

1 Kiminami CS

1Botta F

WJ1and Bolfarini C

1

1

Department of Materials Engineering ndash Federal University of Satildeo CarlosRod Washington Luiz km 235 ndash Satildeo Carlos ndash SP ndash Brazil - CEP 13565-905

Corresponding author moreirapowerufscarbr2Departamento de Ingenieria Mecacircnica - Facultad de Ingenieria - Universidad de Buenos Aires

Av Paseo Coloacuten 850 ndash Buenos Aires BA ndash Argentina

ABSTRACT

A nanostructured aluminium alloy powder prepared by rapid solidification via gas

atomization was consolidated into bulk material under various processing conditions via hot

extrusion The microstructure modifications and mechanical properties of the consolidated alloys as

a function of the extrusion conditions were investigated The increase in the extrusion-load with the

increase of extrusion-rate and decrease of temperature are shown and discussed in association withthe modification in the microstructures The differences in mechanical properties measured by

compressive tests are also discussed in association with the extrusion parameters Furthermore

suggestions are given for rationalising the extrusion ratio and temperature conditions for the

consolidation of nanostructured aluminium alloy powders via hot extrusion

INTRODUCTION

In the last years due to remarkable potentialities in terms of physical and mechanical

properties nanostructured materials have been subject of large amount of research [1ndash3] A variety

of techniques such as mechanical alloying and rapid solidification have been successfully used to prepare nanostructured materials [4] However powders or foils are usually the result of these

materials when they are prepared by the above mentioned methods and thus they cannot be directly

used for structural applications Consequently development of consolidation processes suitable fornanostructured materials are of interest associated mainly with nanostructured powder materials

The published research up to date has shown that extrusion is one of the most effective

processes for the powder materials consolidation [5ndash8] In the present work we investigated the

influence of the two main technical parameters strain rate and temperature of hot extrusion on the

microstructure and mechanical properties of the bulk material consolidated from nanostructured

aluminium alloy powder

MATERIALS AND METHODS

Rapidly solidified aluminium alloy powder with a nominal composition of Al-30Fe-

042Cu-037Mn (wt ) were prepared using argon gas atomisation The nanostructured aluminium

alloy powder with an average grain size of 25 nm microstructure was obtained The nanostructured

powder cylindrical preforms for consolidation processing with a relative density of about 0middot96 and

with initial diameter of 262 mm were prepared by cold pressing The preforms were then

consolidated into 79 mm diameter bars of bulk material by hot extrusion at 3 di983142983142 erent temperatures

375 400 and 425degC with an extrusion ratio of 101 and ram speed of 1 15 and 30 mms

Materials Science Forum Vol 570 (2008) pp 91-96 online at httpwwwscientificnet copy (2008) Trans Tech Publications Switzerland Online available since 2008Feb18

All rights reserved No part of contents of this paper may be repr oduced or transmitted in any form or by any means without the written permission of thepublisher Trans Tech Publications Ltd Switzerland wwwttpnet (ID 14310725255-130808043841)

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 26

The mean extrusion strain rate was calculated using the following equation [9]

where V is the average ram speed DC is the container bore (262mm) DE is the diameter of the

extruded rod (79mm) and α is the dead-metal zone semiangle (60o)

The mechanical properties of the bulk material consolidated from nanostructured aluminium

alloy powder were determined by means of room-temperature compression tests which were

performed using the Interactive Instruments 1k-16 universal testing machine the compression speed

was 05 mmmin

The grain size of the as extruded alloy was characterised by X-ray di983142983142 raction using a Rigaku

diffractometer with Cu K α radiation Microstructural observations were carried out by transmission

electron microscopy (TEM) with a Philips CMndash120 microscope Thin foils for TEM observation

were prepared by ion milling

RESULTS AND DISCUSSION

Grain size and microstructure

To understand the strength and ductility achieved in the processed Al-30Fe-042Cu-037Mn

powder alloy the microstructure and phases constitution of the alloy have been investigated Fig 1

shows a zoom of the XRD pattern after extrusion from samples in three different temperatures Two

phases have been identified from the XRD patterns these are fcc-Al solid solution and Al3Fe One

can observe the substantial fcc-Al peak broadening with decreasing of extrusion temperature

suggesting nanosized fcc-Al grains and the Al3Fe peak contraction and intensity reduction with theextrusion temperature increasing indicating both precipitate coarsening and dissolution

30 35 40 45 50

2θθθθ (deg)

I n t e n s i t y

Al3Fe

375oC

400oC

425oC

Powder

Al3Fe

Figure 1 - XRD patterns of the processed bulk Al-30Fe-042Cu-037Mn powder alloy after

extrusion

Figure 2 shows the average grain size of the bulk aluminium alloy before and after

extrusion as a function of extrusion temperature The value at 25degC is the powder average grain

size The data points were fitted to a representative curve to obtain the approximate behaviour

between 25degC and the other temperatures It is believed that there is a critical temperature for grain

growth during consolidation by hot extrusion When the extrusion temperature is above the critical

one the average grain size of the consolidated alloy quickly increases with the extrusion

temperature increasing reaching about 69 nm at 425degC

The influence of temperature on grain growth rate (GGR) can be expressed in an Arrheniustype equation GGR asymp exp(minusQRT ) where Q is the activation energy for isothermal grain growth

92 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 36

R the molar gas constant and T the absolute temperature

If the grain growth of the nanostructured aluminium alloy during hot extrusion can be

considered as isothermal grain growth then the grain growth behaviour is mainly dependent on two

factors which govern the grain growth rate the activation energy (Q) and the extrusion temperature

(T) From the above equation it is clear that the rate is small when the activation energy is high or

the temperature is decreased Since nanosize grains usually have very high activation energy forgrain growth the GGR has a tendency to be smaller when the nanostructured aluminium alloy

powder undertakes hot extrusion at relatively low temperatures As a result it can be expected that

the grain growth will not be significant when the extrusion temperature is low If the activation

energy is unchanged according to the above equation with the enhancement of the extrusion

temperature the grain growth rate will be increased and thus causing faster grain growth In fact

when the extrusion process is performed within a relatively low temperature range the activation

energy of the nanostructured aluminium alloy will increase with increasing temperature due to the

precipitate effect that pin the grain boundary movement necessary for grain growth and thus when

the extrusion process is carried out at lower temperatures bellow the critical one the GGR can be

kept at relatively lower values and it can be expected that the grain growth is limited to a certain

amount But when the temperature is increased up to the critical value the coarsening anddissolving of the precipitates will occur with the temperature increasing leading to the reduction or

disappearance of the pinning effect of the precipitates and thus decreasing the activation energy

even as the effect of increasing temperature on enhancement of the GGR becomes more important

Therefore when the extrusion process is carried out at temperatures above the critical value the

value of the grain growth quickly increases and the grain growth during extrusion becomes more

remarkable

0

20

40

60

80

100

0 200 400 600

Temperature (C)

G r a i n S i z e ( n m )

Figure 2 - Dependence of the average grain size on extrusion temperature

Figure 3a shows TEM image of the aluminium powder alloy and the selected area electron

diffraction pattern (SAEDP) showing the fcc-Al pattern and the small grain dimension Also the

TEM analysis reveals the presence of small precipitates especially at grain boundaries inferred

from Fig 1 as Al3Fe and that the particle sizes of Al3Fe intermetallic precipitates are similar to thegrain size of fcc-Al all of which averaging about 25 nm Also the volume fraction of these

precipitates is about 8

Figure 3b shows TEM image of the as extruded bulk aluminium alloy consolidated from

nanostructured powder at 425oC and 293 s-1 It appears that the TEM observation of grain size

agrees well with the results of the XRD analysis shown in Fig 2 The main following

microstructural features which correspond to the final extrusion temperatures have been revealed

no obvious precipitation particles can be observed in the bulk material consolidated only in the

powder before the extrusion (Fig 3a) the quantity of the precipitated particles was found to have

reduced significantly indicating the precipitate dissolution and the significant enhancement on the

solubility of the alloying elements in aluminium at that temperature (which agrees with the XRD

pattern shown in Fig 1) Obviously the TEM observation results support the preceding analysis forthe grain growth of the nanostructured aluminium alloy during the extrusion process

Materials Science Forum Vol 570 93

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 46

(a) Powder (25 degC) (b) Extruded (425 degC)

Figure 3 - TEM images of bulk aluminium alloy consolidated at the indicated temperatures

Mechanical properties

Figure 4 shows the dependence of room temperature compressive mechanical properties for

the as extruded alloy on extrusion temperature The elongation of the as extruded alloy tends to

increase with the increasing of the extrusion temperature Also only within the range 375ndash400degC

does the elongation of the consolidated material increased significantly At higher temperatures(400ndash425degC) a small decrease in elongation with increasing temperature was observed As the

elongation of the bulk material consolidated from powders is extremely dependent on the

densification effects of the powder preform and the bonding condition of the alloy powders it is

believed that only when the extrusion temperature is around 400degC good properties for the

consolidated nanostructured aluminium powder can be obtained As for yield compressive strength

σs it has similar dependence on the extrusion temperature When the nanostructured aluminium

alloy powders are extruded at temperatures below 400degC even with the poor bonding of the

powders particles the consolidated material possesses reasonably high strength due to the fact that

grain growth during extrusion is small and due to the hardening effect resulting from the existent

precipitates Yet when the extrusion process is performed within the temperature range 375ndash400degC

the strength of the consolidated material is considerably reduced Perhaps this is a result of thecoherency breakdown between the precipitates and the matrix lattice and the precipitate coarsening

which leads to the disappearance of precipitation hardening The bonding condition of the powders

cannot be enhanced significantly within the temperature range 375ndash400degC When the extrusion tem-

perature is increased to the range 400ndash425degC the consolidated material strength tends to increase

again due to the significant enhancement of the powder bonding condition and the increase in the

alloy elements solubility in the matrix lattice even considering the grain growth that occurred during

the extrusion process

These results suggest that to obtain both high strength and good elongation the temperature

for hot extrusion of these nanostructured aluminium powders should be selected within the range

400ndash425degC when the extrusion temperature is increased above 425degC the strength of the

consolidated material will decrease with increasing temperature due to excessive grain growth

94 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 56

125

130

135

140

145

150

155

160

360 380 400 420 440

Temperature (C)

S t r

e s s σ σσ σ s ( M P a )

10

147

293

0

10

20

30

40

50

60

360 380 400 420 440

Temperature (C)

E l

o n g a t i o n ( )

10

147

293

Figure 4 - Dependence of room temperature compressive mechanical properties on extrusion

temperature

Figure 5 shows the dependence of the room temperature compressive mechanical properties

of the as extruded alloy on the strain rate in all temperature range One can note that both

compressive strength and elongation of the as extruded alloy increase with the increase in the strain

rate Increasing strain rate increases the pressure and the shear deformation that the powdersexperience during extrusion leading to improvement in the powder bonding to the densification

effect For extrusion strain rate higher than 147 s-1 the increase in mechanical properties of the as

extruded alloy is not noticeable This suggests that extrusion ratio of 147 s -1 can ensure good

bonding strength and full densification of the powder material Therefore the appropriate strain rate

for the hot extrusion of the nanostructured aluminium powder is 147 ndash 293 s-1 It can be noticed

that very high strain rate will only cause the rising of the process cost and will not do much to

increase the mechanical properties

110

120

130

140

150

160

0 10 20 30

Strain Rate (1s)

S t r e s s σ σσ σ s

( M P a )

425 C

400 C

375 C

0

10

20

30

40

50

60

0 10 20 30

Strain Rate (1s)

E l o n g a t i o

n ( )

375 C

400 C

425 C

Figure 5 - Dependence of room temperature compressive mechanical properties on extrusion ratio

CONCLUSIONS

The grain growth behaviour of the nanostructured aluminium alloy studied in this work during

extrusion is strongly dependent on the extrusion temperature

The bonding strength of the nanostructured aluminium powder is susceptible to the extrusion

temperature

A larger extrusion ratio is useful to increase the powder bonding strength and the densification

e983142983142 ect as a result both the elongation and the compressive strength of the consolidated material will

give rise to the enhancement

Materials Science Forum Vol 570 95

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III

Page 2: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 26

The mean extrusion strain rate was calculated using the following equation [9]

where V is the average ram speed DC is the container bore (262mm) DE is the diameter of the

extruded rod (79mm) and α is the dead-metal zone semiangle (60o)

The mechanical properties of the bulk material consolidated from nanostructured aluminium

alloy powder were determined by means of room-temperature compression tests which were

performed using the Interactive Instruments 1k-16 universal testing machine the compression speed

was 05 mmmin

The grain size of the as extruded alloy was characterised by X-ray di983142983142 raction using a Rigaku

diffractometer with Cu K α radiation Microstructural observations were carried out by transmission

electron microscopy (TEM) with a Philips CMndash120 microscope Thin foils for TEM observation

were prepared by ion milling

RESULTS AND DISCUSSION

Grain size and microstructure

To understand the strength and ductility achieved in the processed Al-30Fe-042Cu-037Mn

powder alloy the microstructure and phases constitution of the alloy have been investigated Fig 1

shows a zoom of the XRD pattern after extrusion from samples in three different temperatures Two

phases have been identified from the XRD patterns these are fcc-Al solid solution and Al3Fe One

can observe the substantial fcc-Al peak broadening with decreasing of extrusion temperature

suggesting nanosized fcc-Al grains and the Al3Fe peak contraction and intensity reduction with theextrusion temperature increasing indicating both precipitate coarsening and dissolution

30 35 40 45 50

2θθθθ (deg)

I n t e n s i t y

Al3Fe

375oC

400oC

425oC

Powder

Al3Fe

Figure 1 - XRD patterns of the processed bulk Al-30Fe-042Cu-037Mn powder alloy after

extrusion

Figure 2 shows the average grain size of the bulk aluminium alloy before and after

extrusion as a function of extrusion temperature The value at 25degC is the powder average grain

size The data points were fitted to a representative curve to obtain the approximate behaviour

between 25degC and the other temperatures It is believed that there is a critical temperature for grain

growth during consolidation by hot extrusion When the extrusion temperature is above the critical

one the average grain size of the consolidated alloy quickly increases with the extrusion

temperature increasing reaching about 69 nm at 425degC

The influence of temperature on grain growth rate (GGR) can be expressed in an Arrheniustype equation GGR asymp exp(minusQRT ) where Q is the activation energy for isothermal grain growth

92 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 36

R the molar gas constant and T the absolute temperature

If the grain growth of the nanostructured aluminium alloy during hot extrusion can be

considered as isothermal grain growth then the grain growth behaviour is mainly dependent on two

factors which govern the grain growth rate the activation energy (Q) and the extrusion temperature

(T) From the above equation it is clear that the rate is small when the activation energy is high or

the temperature is decreased Since nanosize grains usually have very high activation energy forgrain growth the GGR has a tendency to be smaller when the nanostructured aluminium alloy

powder undertakes hot extrusion at relatively low temperatures As a result it can be expected that

the grain growth will not be significant when the extrusion temperature is low If the activation

energy is unchanged according to the above equation with the enhancement of the extrusion

temperature the grain growth rate will be increased and thus causing faster grain growth In fact

when the extrusion process is performed within a relatively low temperature range the activation

energy of the nanostructured aluminium alloy will increase with increasing temperature due to the

precipitate effect that pin the grain boundary movement necessary for grain growth and thus when

the extrusion process is carried out at lower temperatures bellow the critical one the GGR can be

kept at relatively lower values and it can be expected that the grain growth is limited to a certain

amount But when the temperature is increased up to the critical value the coarsening anddissolving of the precipitates will occur with the temperature increasing leading to the reduction or

disappearance of the pinning effect of the precipitates and thus decreasing the activation energy

even as the effect of increasing temperature on enhancement of the GGR becomes more important

Therefore when the extrusion process is carried out at temperatures above the critical value the

value of the grain growth quickly increases and the grain growth during extrusion becomes more

remarkable

0

20

40

60

80

100

0 200 400 600

Temperature (C)

G r a i n S i z e ( n m )

Figure 2 - Dependence of the average grain size on extrusion temperature

Figure 3a shows TEM image of the aluminium powder alloy and the selected area electron

diffraction pattern (SAEDP) showing the fcc-Al pattern and the small grain dimension Also the

TEM analysis reveals the presence of small precipitates especially at grain boundaries inferred

from Fig 1 as Al3Fe and that the particle sizes of Al3Fe intermetallic precipitates are similar to thegrain size of fcc-Al all of which averaging about 25 nm Also the volume fraction of these

precipitates is about 8

Figure 3b shows TEM image of the as extruded bulk aluminium alloy consolidated from

nanostructured powder at 425oC and 293 s-1 It appears that the TEM observation of grain size

agrees well with the results of the XRD analysis shown in Fig 2 The main following

microstructural features which correspond to the final extrusion temperatures have been revealed

no obvious precipitation particles can be observed in the bulk material consolidated only in the

powder before the extrusion (Fig 3a) the quantity of the precipitated particles was found to have

reduced significantly indicating the precipitate dissolution and the significant enhancement on the

solubility of the alloying elements in aluminium at that temperature (which agrees with the XRD

pattern shown in Fig 1) Obviously the TEM observation results support the preceding analysis forthe grain growth of the nanostructured aluminium alloy during the extrusion process

Materials Science Forum Vol 570 93

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 46

(a) Powder (25 degC) (b) Extruded (425 degC)

Figure 3 - TEM images of bulk aluminium alloy consolidated at the indicated temperatures

Mechanical properties

Figure 4 shows the dependence of room temperature compressive mechanical properties for

the as extruded alloy on extrusion temperature The elongation of the as extruded alloy tends to

increase with the increasing of the extrusion temperature Also only within the range 375ndash400degC

does the elongation of the consolidated material increased significantly At higher temperatures(400ndash425degC) a small decrease in elongation with increasing temperature was observed As the

elongation of the bulk material consolidated from powders is extremely dependent on the

densification effects of the powder preform and the bonding condition of the alloy powders it is

believed that only when the extrusion temperature is around 400degC good properties for the

consolidated nanostructured aluminium powder can be obtained As for yield compressive strength

σs it has similar dependence on the extrusion temperature When the nanostructured aluminium

alloy powders are extruded at temperatures below 400degC even with the poor bonding of the

powders particles the consolidated material possesses reasonably high strength due to the fact that

grain growth during extrusion is small and due to the hardening effect resulting from the existent

precipitates Yet when the extrusion process is performed within the temperature range 375ndash400degC

the strength of the consolidated material is considerably reduced Perhaps this is a result of thecoherency breakdown between the precipitates and the matrix lattice and the precipitate coarsening

which leads to the disappearance of precipitation hardening The bonding condition of the powders

cannot be enhanced significantly within the temperature range 375ndash400degC When the extrusion tem-

perature is increased to the range 400ndash425degC the consolidated material strength tends to increase

again due to the significant enhancement of the powder bonding condition and the increase in the

alloy elements solubility in the matrix lattice even considering the grain growth that occurred during

the extrusion process

These results suggest that to obtain both high strength and good elongation the temperature

for hot extrusion of these nanostructured aluminium powders should be selected within the range

400ndash425degC when the extrusion temperature is increased above 425degC the strength of the

consolidated material will decrease with increasing temperature due to excessive grain growth

94 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 56

125

130

135

140

145

150

155

160

360 380 400 420 440

Temperature (C)

S t r

e s s σ σσ σ s ( M P a )

10

147

293

0

10

20

30

40

50

60

360 380 400 420 440

Temperature (C)

E l

o n g a t i o n ( )

10

147

293

Figure 4 - Dependence of room temperature compressive mechanical properties on extrusion

temperature

Figure 5 shows the dependence of the room temperature compressive mechanical properties

of the as extruded alloy on the strain rate in all temperature range One can note that both

compressive strength and elongation of the as extruded alloy increase with the increase in the strain

rate Increasing strain rate increases the pressure and the shear deformation that the powdersexperience during extrusion leading to improvement in the powder bonding to the densification

effect For extrusion strain rate higher than 147 s-1 the increase in mechanical properties of the as

extruded alloy is not noticeable This suggests that extrusion ratio of 147 s -1 can ensure good

bonding strength and full densification of the powder material Therefore the appropriate strain rate

for the hot extrusion of the nanostructured aluminium powder is 147 ndash 293 s-1 It can be noticed

that very high strain rate will only cause the rising of the process cost and will not do much to

increase the mechanical properties

110

120

130

140

150

160

0 10 20 30

Strain Rate (1s)

S t r e s s σ σσ σ s

( M P a )

425 C

400 C

375 C

0

10

20

30

40

50

60

0 10 20 30

Strain Rate (1s)

E l o n g a t i o

n ( )

375 C

400 C

425 C

Figure 5 - Dependence of room temperature compressive mechanical properties on extrusion ratio

CONCLUSIONS

The grain growth behaviour of the nanostructured aluminium alloy studied in this work during

extrusion is strongly dependent on the extrusion temperature

The bonding strength of the nanostructured aluminium powder is susceptible to the extrusion

temperature

A larger extrusion ratio is useful to increase the powder bonding strength and the densification

e983142983142 ect as a result both the elongation and the compressive strength of the consolidated material will

give rise to the enhancement

Materials Science Forum Vol 570 95

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III

Page 3: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 36

R the molar gas constant and T the absolute temperature

If the grain growth of the nanostructured aluminium alloy during hot extrusion can be

considered as isothermal grain growth then the grain growth behaviour is mainly dependent on two

factors which govern the grain growth rate the activation energy (Q) and the extrusion temperature

(T) From the above equation it is clear that the rate is small when the activation energy is high or

the temperature is decreased Since nanosize grains usually have very high activation energy forgrain growth the GGR has a tendency to be smaller when the nanostructured aluminium alloy

powder undertakes hot extrusion at relatively low temperatures As a result it can be expected that

the grain growth will not be significant when the extrusion temperature is low If the activation

energy is unchanged according to the above equation with the enhancement of the extrusion

temperature the grain growth rate will be increased and thus causing faster grain growth In fact

when the extrusion process is performed within a relatively low temperature range the activation

energy of the nanostructured aluminium alloy will increase with increasing temperature due to the

precipitate effect that pin the grain boundary movement necessary for grain growth and thus when

the extrusion process is carried out at lower temperatures bellow the critical one the GGR can be

kept at relatively lower values and it can be expected that the grain growth is limited to a certain

amount But when the temperature is increased up to the critical value the coarsening anddissolving of the precipitates will occur with the temperature increasing leading to the reduction or

disappearance of the pinning effect of the precipitates and thus decreasing the activation energy

even as the effect of increasing temperature on enhancement of the GGR becomes more important

Therefore when the extrusion process is carried out at temperatures above the critical value the

value of the grain growth quickly increases and the grain growth during extrusion becomes more

remarkable

0

20

40

60

80

100

0 200 400 600

Temperature (C)

G r a i n S i z e ( n m )

Figure 2 - Dependence of the average grain size on extrusion temperature

Figure 3a shows TEM image of the aluminium powder alloy and the selected area electron

diffraction pattern (SAEDP) showing the fcc-Al pattern and the small grain dimension Also the

TEM analysis reveals the presence of small precipitates especially at grain boundaries inferred

from Fig 1 as Al3Fe and that the particle sizes of Al3Fe intermetallic precipitates are similar to thegrain size of fcc-Al all of which averaging about 25 nm Also the volume fraction of these

precipitates is about 8

Figure 3b shows TEM image of the as extruded bulk aluminium alloy consolidated from

nanostructured powder at 425oC and 293 s-1 It appears that the TEM observation of grain size

agrees well with the results of the XRD analysis shown in Fig 2 The main following

microstructural features which correspond to the final extrusion temperatures have been revealed

no obvious precipitation particles can be observed in the bulk material consolidated only in the

powder before the extrusion (Fig 3a) the quantity of the precipitated particles was found to have

reduced significantly indicating the precipitate dissolution and the significant enhancement on the

solubility of the alloying elements in aluminium at that temperature (which agrees with the XRD

pattern shown in Fig 1) Obviously the TEM observation results support the preceding analysis forthe grain growth of the nanostructured aluminium alloy during the extrusion process

Materials Science Forum Vol 570 93

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 46

(a) Powder (25 degC) (b) Extruded (425 degC)

Figure 3 - TEM images of bulk aluminium alloy consolidated at the indicated temperatures

Mechanical properties

Figure 4 shows the dependence of room temperature compressive mechanical properties for

the as extruded alloy on extrusion temperature The elongation of the as extruded alloy tends to

increase with the increasing of the extrusion temperature Also only within the range 375ndash400degC

does the elongation of the consolidated material increased significantly At higher temperatures(400ndash425degC) a small decrease in elongation with increasing temperature was observed As the

elongation of the bulk material consolidated from powders is extremely dependent on the

densification effects of the powder preform and the bonding condition of the alloy powders it is

believed that only when the extrusion temperature is around 400degC good properties for the

consolidated nanostructured aluminium powder can be obtained As for yield compressive strength

σs it has similar dependence on the extrusion temperature When the nanostructured aluminium

alloy powders are extruded at temperatures below 400degC even with the poor bonding of the

powders particles the consolidated material possesses reasonably high strength due to the fact that

grain growth during extrusion is small and due to the hardening effect resulting from the existent

precipitates Yet when the extrusion process is performed within the temperature range 375ndash400degC

the strength of the consolidated material is considerably reduced Perhaps this is a result of thecoherency breakdown between the precipitates and the matrix lattice and the precipitate coarsening

which leads to the disappearance of precipitation hardening The bonding condition of the powders

cannot be enhanced significantly within the temperature range 375ndash400degC When the extrusion tem-

perature is increased to the range 400ndash425degC the consolidated material strength tends to increase

again due to the significant enhancement of the powder bonding condition and the increase in the

alloy elements solubility in the matrix lattice even considering the grain growth that occurred during

the extrusion process

These results suggest that to obtain both high strength and good elongation the temperature

for hot extrusion of these nanostructured aluminium powders should be selected within the range

400ndash425degC when the extrusion temperature is increased above 425degC the strength of the

consolidated material will decrease with increasing temperature due to excessive grain growth

94 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 56

125

130

135

140

145

150

155

160

360 380 400 420 440

Temperature (C)

S t r

e s s σ σσ σ s ( M P a )

10

147

293

0

10

20

30

40

50

60

360 380 400 420 440

Temperature (C)

E l

o n g a t i o n ( )

10

147

293

Figure 4 - Dependence of room temperature compressive mechanical properties on extrusion

temperature

Figure 5 shows the dependence of the room temperature compressive mechanical properties

of the as extruded alloy on the strain rate in all temperature range One can note that both

compressive strength and elongation of the as extruded alloy increase with the increase in the strain

rate Increasing strain rate increases the pressure and the shear deformation that the powdersexperience during extrusion leading to improvement in the powder bonding to the densification

effect For extrusion strain rate higher than 147 s-1 the increase in mechanical properties of the as

extruded alloy is not noticeable This suggests that extrusion ratio of 147 s -1 can ensure good

bonding strength and full densification of the powder material Therefore the appropriate strain rate

for the hot extrusion of the nanostructured aluminium powder is 147 ndash 293 s-1 It can be noticed

that very high strain rate will only cause the rising of the process cost and will not do much to

increase the mechanical properties

110

120

130

140

150

160

0 10 20 30

Strain Rate (1s)

S t r e s s σ σσ σ s

( M P a )

425 C

400 C

375 C

0

10

20

30

40

50

60

0 10 20 30

Strain Rate (1s)

E l o n g a t i o

n ( )

375 C

400 C

425 C

Figure 5 - Dependence of room temperature compressive mechanical properties on extrusion ratio

CONCLUSIONS

The grain growth behaviour of the nanostructured aluminium alloy studied in this work during

extrusion is strongly dependent on the extrusion temperature

The bonding strength of the nanostructured aluminium powder is susceptible to the extrusion

temperature

A larger extrusion ratio is useful to increase the powder bonding strength and the densification

e983142983142 ect as a result both the elongation and the compressive strength of the consolidated material will

give rise to the enhancement

Materials Science Forum Vol 570 95

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III

Page 4: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 46

(a) Powder (25 degC) (b) Extruded (425 degC)

Figure 3 - TEM images of bulk aluminium alloy consolidated at the indicated temperatures

Mechanical properties

Figure 4 shows the dependence of room temperature compressive mechanical properties for

the as extruded alloy on extrusion temperature The elongation of the as extruded alloy tends to

increase with the increasing of the extrusion temperature Also only within the range 375ndash400degC

does the elongation of the consolidated material increased significantly At higher temperatures(400ndash425degC) a small decrease in elongation with increasing temperature was observed As the

elongation of the bulk material consolidated from powders is extremely dependent on the

densification effects of the powder preform and the bonding condition of the alloy powders it is

believed that only when the extrusion temperature is around 400degC good properties for the

consolidated nanostructured aluminium powder can be obtained As for yield compressive strength

σs it has similar dependence on the extrusion temperature When the nanostructured aluminium

alloy powders are extruded at temperatures below 400degC even with the poor bonding of the

powders particles the consolidated material possesses reasonably high strength due to the fact that

grain growth during extrusion is small and due to the hardening effect resulting from the existent

precipitates Yet when the extrusion process is performed within the temperature range 375ndash400degC

the strength of the consolidated material is considerably reduced Perhaps this is a result of thecoherency breakdown between the precipitates and the matrix lattice and the precipitate coarsening

which leads to the disappearance of precipitation hardening The bonding condition of the powders

cannot be enhanced significantly within the temperature range 375ndash400degC When the extrusion tem-

perature is increased to the range 400ndash425degC the consolidated material strength tends to increase

again due to the significant enhancement of the powder bonding condition and the increase in the

alloy elements solubility in the matrix lattice even considering the grain growth that occurred during

the extrusion process

These results suggest that to obtain both high strength and good elongation the temperature

for hot extrusion of these nanostructured aluminium powders should be selected within the range

400ndash425degC when the extrusion temperature is increased above 425degC the strength of the

consolidated material will decrease with increasing temperature due to excessive grain growth

94 Metastable and Nanostructured Materials III

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 56

125

130

135

140

145

150

155

160

360 380 400 420 440

Temperature (C)

S t r

e s s σ σσ σ s ( M P a )

10

147

293

0

10

20

30

40

50

60

360 380 400 420 440

Temperature (C)

E l

o n g a t i o n ( )

10

147

293

Figure 4 - Dependence of room temperature compressive mechanical properties on extrusion

temperature

Figure 5 shows the dependence of the room temperature compressive mechanical properties

of the as extruded alloy on the strain rate in all temperature range One can note that both

compressive strength and elongation of the as extruded alloy increase with the increase in the strain

rate Increasing strain rate increases the pressure and the shear deformation that the powdersexperience during extrusion leading to improvement in the powder bonding to the densification

effect For extrusion strain rate higher than 147 s-1 the increase in mechanical properties of the as

extruded alloy is not noticeable This suggests that extrusion ratio of 147 s -1 can ensure good

bonding strength and full densification of the powder material Therefore the appropriate strain rate

for the hot extrusion of the nanostructured aluminium powder is 147 ndash 293 s-1 It can be noticed

that very high strain rate will only cause the rising of the process cost and will not do much to

increase the mechanical properties

110

120

130

140

150

160

0 10 20 30

Strain Rate (1s)

S t r e s s σ σσ σ s

( M P a )

425 C

400 C

375 C

0

10

20

30

40

50

60

0 10 20 30

Strain Rate (1s)

E l o n g a t i o

n ( )

375 C

400 C

425 C

Figure 5 - Dependence of room temperature compressive mechanical properties on extrusion ratio

CONCLUSIONS

The grain growth behaviour of the nanostructured aluminium alloy studied in this work during

extrusion is strongly dependent on the extrusion temperature

The bonding strength of the nanostructured aluminium powder is susceptible to the extrusion

temperature

A larger extrusion ratio is useful to increase the powder bonding strength and the densification

e983142983142 ect as a result both the elongation and the compressive strength of the consolidated material will

give rise to the enhancement

Materials Science Forum Vol 570 95

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III

Page 5: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 56

125

130

135

140

145

150

155

160

360 380 400 420 440

Temperature (C)

S t r

e s s σ σσ σ s ( M P a )

10

147

293

0

10

20

30

40

50

60

360 380 400 420 440

Temperature (C)

E l

o n g a t i o n ( )

10

147

293

Figure 4 - Dependence of room temperature compressive mechanical properties on extrusion

temperature

Figure 5 shows the dependence of the room temperature compressive mechanical properties

of the as extruded alloy on the strain rate in all temperature range One can note that both

compressive strength and elongation of the as extruded alloy increase with the increase in the strain

rate Increasing strain rate increases the pressure and the shear deformation that the powdersexperience during extrusion leading to improvement in the powder bonding to the densification

effect For extrusion strain rate higher than 147 s-1 the increase in mechanical properties of the as

extruded alloy is not noticeable This suggests that extrusion ratio of 147 s -1 can ensure good

bonding strength and full densification of the powder material Therefore the appropriate strain rate

for the hot extrusion of the nanostructured aluminium powder is 147 ndash 293 s-1 It can be noticed

that very high strain rate will only cause the rising of the process cost and will not do much to

increase the mechanical properties

110

120

130

140

150

160

0 10 20 30

Strain Rate (1s)

S t r e s s σ σσ σ s

( M P a )

425 C

400 C

375 C

0

10

20

30

40

50

60

0 10 20 30

Strain Rate (1s)

E l o n g a t i o

n ( )

375 C

400 C

425 C

Figure 5 - Dependence of room temperature compressive mechanical properties on extrusion ratio

CONCLUSIONS

The grain growth behaviour of the nanostructured aluminium alloy studied in this work during

extrusion is strongly dependent on the extrusion temperature

The bonding strength of the nanostructured aluminium powder is susceptible to the extrusion

temperature

A larger extrusion ratio is useful to increase the powder bonding strength and the densification

e983142983142 ect as a result both the elongation and the compressive strength of the consolidated material will

give rise to the enhancement

Materials Science Forum Vol 570 95

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III

Page 6: Hot Extrusion of Nanostructured Al Alloy Powder: Extrusion Ratio and Temperature Effect on the Microstructure and Mechanical Properties

8102019 Hot Extrusion of Nanostructured Al Alloy Powder Extrusion Ratio and Temperature Effect on the Microstructure anhellip

httpslidepdfcomreaderfullhot-extrusion-of-nanostructured-al-alloy-powder-extrusion-ratio-and-temperature 66

REFERENCES

1 - J B Fogagnolo M H Robert E M Ruiz-Navas and M Torralba Journal of Materials

Science 2002 37 4603 ndash 4607

2 - L Ma T F Zahrah R Fields - Processing And Simulation Of Consolidation Of

Amorphous Aluminum-Based Powder Material in Proceedings of IMECrsquo03 2003 ASMEIntern Mech Eng Cong Washington DC Nov 15-21 2003

3 - MD Salvador V Amigoacute N Martinez DJ Busquets Journal of Materials Processing

Technology 2003 143ndash144 605ndash611

4 - C Suryanarayana Int Mater Rev 1995 40 (2) 41

5 - L Hu Z Li and E Wang Powder Metallurgy 1999 Vol 42 No 2 153

6 - K Ohuchi And H J Takahash Bull Jpn Inst Met 1983 47 ( 3) 258

7 - N Inoue And M Nishara lsquoHydrostatic Extrusion ndash Theory And Applicationrsquo 1985

Oxford Elsevier

8 - Z Li Et Al Chin J Nonferrous Met 1995 5 ( 4) 102

9 - AF Castle and T Sheppard Hot Working Theory Applied to Extrusion of Some Aluminum

Alloys Met Technol 1976 3 (10) 1976

96 Metastable and Nanostructured Materials III