Grain Refinement of Al -Si Alloys by Nb-B Inoculation. Part 1: - - PowerPoint PPT Presentation

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Grain Refinement of Al -Si Alloys by Nb-B Inoculation. Part 1: Concept Development and Effect on Binary Alloys. Part 2: Application to Commercial Alloys 1 Grain refinement of Al-Si alloys by Nb-B inoculation M. Nowak L. Bolzoni N. Hari

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SLIDE 1

“Grain Refinement of Al-Si Alloys by Nb-B Inoculation. Part 1: Concept Development and Effect on Binary Alloys. Part 2: Application to Commercial Alloys”

1

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SLIDE 2

Grain refinement of Al-Si alloys by Nb-B inoculation

  • M. Nowak
  • L. Bolzoni
  • N. Hari Babu

Brunel Centre for Advanced Solidification Technology

Brunel University London, UK

The Charles Hatchett Award 2016 Lecture

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SLIDE 3

Outline

  • Grain refinement in Al alloys with Al-5Ti-B
  • Concept development
  • Application to Al-Si cast alloys
  • Al-Nb-B master alloy
  • Comparative study between Al-Nb-B and Al-5Ti-B master alloys

The Charles Hatchett Award 2016 Lecture

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SLIDE 4

ALUMINIUM ALLOYS

INTRODUCTION

PROPERTIES

  • LOW DENSITY, 2.7 g/cc
  • GOOD MECHANICAL PROPERTIES
  • HIGH CORROSION RESISTANCE
  • HIGH THERMAL CONDUCTIVITY
  • LOW ELECTRICAL RESISTIVITY

WROUGHT ALLOYS GRAIN REFINEMENT IMPROVEMENT

FLUIDITY/CASTABILITY MECHANICAL PROPERTIES MACHINABILITY SURFACE QUALITY CHEMICAL HOMOGENEITY REDUCED SHRINKAGE POROSITY

CAST (Al-Si)

The Charles Hatchett Award 2016 Lecture

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SLIDE 5

Factors determining grain size in as cast microstructure

Nucleation & Growth

Heterogeneous nucleation Homogeneous nucleation Growth Kinetics

  • Temperature
  • Atmosphere/Pressure
  • Growth restriction
  • Fragmentation
  • Cooling rate

Under cooling (DT)

Nucleation / growth rate DT = TL-Tg

TL

The Charles Hatchett Award 2016 Lecture

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SLIDE 6

EFFICIENT HETEROGENEOUS NUCLEATION SITES

1. High melting Temp 2. Low lattice mismatch (atom position matching)

  • 3. Chemical stability

(should not react with alloying elements)

A B A

BASE MATERIAL

  • N. Hari Babu et al., Nature Materials 2005;4:476

The Charles Hatchett Award 2016 Lecture

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SLIDE 7

GRAIN REFINEMENT: Al-Ti-B

Al-Ti-C

MODIFICATION:

Sr modification of the Si morphology P to nucleate the primary Si particles

GRAIN REFINERS IN ALUMINIUM INDUSTRY

TiB2 Particle Al3Ti Layer Al Nuclei

HREM image of Al/Al3Ti/TiB2 interface

  • Orientation Relationships

{111}Al//{112}Al3Ti//{001}TiB2 <110>Al//<201>Al3Ti <110>Al3Ti//<110>TiB2

Source: B. J McKay

The Charles Hatchett Award 2016 Lecture TiB2 & Al3Ti

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SLIDE 8

Mats Johnsson Patent, 2000

Casting alloys Wrought alloys

Influence of Al-Ti-B grain refiner for Al-Si alloys

Ti-Si phase formation Not effective

  • M. Johnsson, Influence of Si And Fe on the Grain-Refinement of

Aluminum, Zeitschrift für Metallkunde, 85 (1994), 781-785

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SLIDE 9

Ti reaction with Si in Al-Si alloys

Ti is consumed by the formation of TiSi2 and TiSi

  • T. E. Quested et al, Mater. Sci.
  • Technol. 22, 1126 (2006)

The Charles Hatchett Award 2016 Lecture

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SLIDE 10

Analogy between Al-Ti & Al-Nb phase diagrams

Al3Ti Al3Nb The Charles Hatchett Award 2016 Lecture

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SLIDE 11

LATTICE MISMATCH

0.384 nm

Al Al (face centred cubic)

Al3Nb

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SLIDE 12

Lattice mismatch ~0.9%

Low Lattice Mismatch – Coherent Interface

The Charles Hatchett Award 2016 Lecture

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SLIDE 13

Nb–Ti–Si ternary system Nb silicides form at higher temperature than Ti silicides thus preventing poisoning Nb–Si binary phase diagram

J.L. Muray and A. J. Alister, Bulletin

  • f Alloy Phase Diagrams 1984;5:74

Nb chemical stability with Si

J.C. Zhao et al., Materials Science and Engineering A 2004;372:21

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SLIDE 14

Al-Nb 660 °C

20 mm

200 μm

Al matrix Nb particles

Addition of Nb metal powder to liquid Al

Unreacted Nb metallic particulates The Charles Hatchett Award 2016 Lecture 750 - 800 C

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SLIDE 15

Nb2Al Nb3Al

Nb NbAl3 Nb3Al Nb2Al

20 μm

Requires high temperature for larger Nb particles and high concentrations

Poor dissolution of Nb in liquid Al

The Charles Hatchett Award 2016 Lecture

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SLIDE 16

Addition of Nb fine metal powder to liquid Al

<45 mm Nb- Superconductivity – 9K To verify the Nb dissolution, magnetic moment vs temperature measured The Charles Hatchett Award 2016 Lecture

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SLIDE 17

700ºC

CP-Aluminium Al with Nb-B

EFFECT OF Nb on CP Al

The Charles Hatchett Award 2016 Lecture

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SLIDE 18

COMPARISON OF Al-Ti-B AND Nb-B ON CP Al

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SLIDE 19

Al-1Si

Reference

Al-2Si Al-10Si Al-8Si Al-6Si Al-5Si Al-4Si

0.1wt.% Al-5Ti-1B 0.1wt.% Nb & B (powders)

COMPARISON OF Al-Ti-B AND Nb-B TO HYPOEUTECTIC BINARY Al-Si Alloys

The Charles Hatchett Award 2016 Lecture

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SLIDE 20

COMPARISON OF Al-Ti-B AND Nb-B TO HYPOEUTECTIC BINARY Al-Si Alloys

Practical alloys composition

700ºC

The Charles Hatchett Award 2016 Lecture

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SLIDE 21

Al-Si alloys for automotive applications

Engine & transmission Components Crankcases Cylinder heads Intake manifolds Housings manual/automatic transmissions Housings power transfer units Chassis Components Subframes Knuckles Steering housings Structural Components Body structures Instrument panels Door frames Wheels VW Source: VW VW HL VW

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ΔTRef = 2.1ºC Undercooling for Al-10Si alloy

The Charles Hatchett Award 2016 Lecture 0.3 oC/s

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SLIDE 23

Grain size up to 1 cm Reference

ΔTRef = 2.1ºC

The Charles Hatchett Award 2016 Lecture

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SLIDE 24

ΔTNb-B = 1.3ºC Undercooling in the presence of NbB2/Al3Nb

The Charles Hatchett Award 2016 Lecture 0.3 oC/s

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SLIDE 25

Grain size up to 1 cm Reference Nb-B Grain size: 2-3 mm

ΔTNb-B = 1.3ºC ΔTRef = 2.1ºC GRAIN STRUCTURE

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380 400 420 440 460 480 500 520 540 580 581 582 583 584 585 586 587 588 589 590 591 592 593 594 595 596 597 598 599 600

LM6 dT/dt Time [ s ] Temerature [

  • C ]
  • 3
  • 2
  • 1

1

dT/dt

Trec

T nucl =588 0 C

T min =584.5 0 C T g =5870 C ΔT=2.5°C

400 420 440 460 480 500 585 586 587 588 589 590 591 592 593 594 595

LM6+NGR dT/dt Time [ s ] Temeprature [

  • C ]
  • 0.6
  • 0.5
  • 0.4
  • 0.3
  • 0.2
  • 0.1

0.0 0.1 0.2

dT/dt

T nucl =588.8 0 C T min =586.8 0 C T g =587.5 0 C ΔT=0.7°C a) b)

Cooling curves for Al-11Si (LM6) alloy

LM6

20 mm LM6 with Grain refiner addition

Nb-B

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SLIDE 27

200 μm

α-Al dendrite

200 μm

α-Al dendrite

HYPEREUTECTIC BINARY Al-Si ALLOYS

Al-14Si 700ºC

The Charles Hatchett Award 2016 Lecture

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SLIDE 28

HYPEREUTECTIC BINARY Al-Si ALLOYS - EUTECTIC

20 μm 20 μm 20 μm 20 μm 20 μm 20 μm

Al-16Si Al-18Si Al-27Si

700ºC

The Charles Hatchett Award 2016 Lecture

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SLIDE 29

200 μm 200 μm 200 μm 200 μm 200 μm 200 μm

HYPEREUTECTIC BINARY Al-Si ALLOYS – PRIMARY SI

Al-16Si Al-18Si Al-27Si

The Charles Hatchett Award 2016 Lecture

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SLIDE 30

Application of Nb-B grain refiner to Al-Si commercial alloys

The Charles Hatchett Award 2016 Lecture

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Commercial alloys tested with Nb-B

GB USA Si Mg Mn Cu Ni Zn Fe LM6 A413 10.0-13.0 0.1max 0.5max 0.1max 0.1max 0.1max 0.6max LM13 336 10.0-13.0 0.2-0.4 0.5max 0.7-1.5 1.5max 0.1max 1max LM24 A380 7.5-9.5 3 max 0.5max 3.0-4.0 0.5 3 1.3max LM25 A356 6.5-7.5 0.2-0.6 0.3 0.2 0.1 0.1 0.5 9.99 0.005 0.005 0.0017 0.0044 0.005 0.09 10.98 0.268 0.21 2.134 0.068 0.778 0.83 6.06 0.275 0.265 2.725 0.0257 0.305 0.356 11.9 0.8 0.005 3.7 2 0.003 0.12

The Charles Hatchett Award 2016 Lecture

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Nb-B Grain Refiner for Al-Si cast alloys Highly effective for Al-Si alloys & Mg alloys

Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 33

500 μm 500 μm 500 μm 500 μm 500 μm 500 μm 500 μm 500 μm 500 μm

LM25 LM6 LM24

Reference Nb-B Al-5Ti-1B

COMMERCIAL HYPOEUTECTIC Al-Si ALLOYS

650ºC

100 200 300 400 500 600 700 800 900 600 610 620 630 640 650 660 670 680 690

α-Al grain size [µm] Pouring temperature [°C]

REFERENCE Nb-B Al-5Ti-1B LM25 LM24 LM6

The Charles Hatchett Award 2016 Lecture

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SLIDE 34

Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys

Fine & uniform grain structure

Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 35

Porosity Al-11Si (LM6) no addition

Al-11Si (LM6) with Nb-B 10 mm

~200mm

~1200mm

~160mm ~200mm

The Charles Hatchett Award 2016 Lecture

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SLIDE 36

Al-Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure

Grain size is less sensitive to cooling rate

Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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EFFECT OF COOLING RATE

20 mm 20 mm

700ºC

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d = 2072 (dT/dt)-0.34 d = 514 (dT/dt)-0.14 500 1000 1500 2000 2500 3000 3500 4000 4500 20 40 60 80 100

α-Al grain size, d [µm] Cooling rate, dT/dt[°C/s]

Reference Nb-B inoculation 100 1000 10000 0.1 10 1000

α-Al grain size, d [µm] Cooling rate, dT/dt[°C/s]

EFFECT OF COOLING RATE

The Charles Hatchett Award 2016 Lecture

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SLIDE 39

EFFECT OF COOLING RATE

0.00E+00 5.00E+09 1.00E+10 1.50E+10 2.00E+10 2.50E+10 3.00E+10 3.50E+10 100 200 300 400 500 600 700 800 900 1000 20 40 60 80 100

Number of grains, Nv [m-3] ΔNv / Nvref [%] Cooling rate, dT/dt[°C/s]

Nv(ref) Nv(Nb-B inoculation) ΔNv ΔNv / Nv(ref)

The Charles Hatchett Award 2016 Lecture

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SLIDE 40

Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate

Highly effective in sand casting cooling conditions

Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 41

REFERENCE Al-Nb-B ADDITION

Al-9Si-2Cu-0.7Mg-0.15Fe

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Al-9Si-2Cu

Alloy Condn. %Cu %Mg %Si %Fe %Mn %Ni %Zn %Pb %Sn %Ti %Sr A354 CAST 1.60-2.0 0.50- 0.60 8.6-9.44 0.154 0.05- 0.10 0.054 0.10 0.014 0.054 0.10- 0.154 0.02- 0.030

The Charles Hatchett Award 2016 Lecture

A354

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Al-Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions

Reduced porosity & macro defects

Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 44

Reduced Macro-porosity with Nb-B

Al-11Si (LM6)

with Al-5Ti-B

with Nb-B

1 mm

1000µm 1000µm

1 mm 1 mm

The Charles Hatchett Award 2016 Lecture

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SLIDE 45

Aluminium Al-Ti-B Novel grain refiner 50000 100000 150000 200000

Porosity Porosity [ mm

2 ]

Reduced porosity in Nb-B grain refiner added castings

Porosity

Tp1 test 700 OC Al-7Si alloy Al-7Si+Al-5Ti-B Al-7Si + Nb-B ~ /cm2

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SLIDE 46

Without With Nb-B addition Fine grain structure Reduced porosity

Al-7Si alloy

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Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects

Fine eutectic structure & intermetallics

Improved ductility & strength Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 48

Fine eutectic structure

Al-11Si (LM6) with Nb-B

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Cooling rate [ C/s] Eutectic Si [µm] LM6 (Reference) LM6 + Nb-B

HPDC

Finer Eutectic Si - wider range of cooling rates

20 μm 20 μm

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SLIDE 50

Al-10Si With Nb-B

The Charles Hatchett Award 2016 Lecture

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SLIDE 51

Reference (Al-13Si) with Nb-B

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SLIDE 52

Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics

Improved ductility & strength

Tolerant to Fe contamination Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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SLIDE 53

2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 170 180 190 200 210 220 230 240

LM6 LM6+Nb-B UTS [ MPa ] Elongation [ % ] Gravity mould Melting temp: 800

  • C

Casting temp: 800

  • C

Improved strength & ductility

Machined from cast bars Improved

  • Crash performance
  • Fatigue performance

yield 82.4 Mpa  102 Mpa Al-11Si alloy The Charles Hatchett Award 2016 Lecture

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SLIDE 54

Al-13Si piston alloy

The Charles Hatchett Award 2016 Lecture Al-Nb-B

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SLIDE 55

Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength

Tolerant to Fe contamination

Recycling of Al-Si scrap The Charles Hatchett Award 2016 Lecture

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Control of Fe-intermetallics in Al scrap

1% Fe Grain refiner to control Al-Fe-Si intermetallics Al5FeSi Al-Fe-Si large needle structure detrimental to mechanical properties A354 A354 + 1%Fe + 0.1%Nb-B

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SLIDE 57

140 150 160 170 180 190 200 0.5 1 1.5 2

Elongation, 4D (%)

Virgin alloy with 1 wt% Fe impurity

Reduced properties due to larger, needle structured intermetallics

UTS (MPa)

Properties recovery through refinement of intermetallics

Virgin alloy

Recovery of properties in Fe-rich aluminium scrap

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SLIDE 58

Nb-B Grain Refiner for Al-Si cast alloys

Highly effective for Al-Si alloys & Mg alloys Fine & uniform grain structure Grain size is less sensitive to cooling rate Highly effective in sand casting cooling conditions Reduced porosity & macro defects Fine eutectic structure & intermetallics Improved ductility & strength Tolerant to Fe contamination

Re-melting & Fading study

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SLIDE 59

FADING STUDY

680ºC

d = 1.12 (t) + 340 R² = 0.95 200 400 600 800 1000 1200 30 60 90 120 150 180 210 240 270

Grain size, d [µm]

Contact time, t [min]

LM6 The Charles Hatchett Award 2016 Lecture

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SLIDE 60

REQUIRED TIME TO SEDIMENT/FADE

2 4 6 8 10 12 14 16 18 20 10 20 30 40 50

Sedimentation height, h [cm] Contact time, t [h]

NbB2 Al3Nb AlB2 20 µm 15 µm 10 µm

Φ or ρ

The Charles Hatchett Award 2016 Lecture

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SLIDE 61

No addition

Al-Nb-B Addition ~ 3-4 mm

Remelting Al-9Si-1.5Cu-0.6Mg-0.15Fe / RE-MELT

1st Re-Melt 2nd Re-Melt 3rd Re-Melt 4th Re-Melt

The Charles Hatchett Award 2016 Lecture

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SLIDE 62

MASTER ALLOY DEVELOPMENT

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SLIDE 63

Al-Nb-B Master Alloy

The Charles Hatchett Award 2016 Lecture

  • 1. Nb metallic powder

+ KBF4

  • 2. Addition of Nb metallic

powder to diluted Al-B master alloy

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MASTER ALLOY (METHOD 1)

Al B Nb Al B Nb Al Al Nb Nb B B Al3Nb NbB2 Al = 68.17 at.% Nb = 26.43 at.% O = 5.40 at.%

The Charles Hatchett Award 2016 Lecture

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Al-2Nb-2B (METHOD 2)

AlB2-12 NbB2 Al3Nb

The Charles Hatchett Award 2016 Lecture

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Al-4Nb-1B ON LM25

Reference Nb-B (M.A.) Al-Nb-B (powders) 680ºC

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SLIDE 67

Al-4Nb-1B ON LM6

680ºC

The Charles Hatchett Award 2016 Lecture

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Al-2Nb-1B ON Al-10Si

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SLIDE 69

EFFECT OF Al-2Nb-2B ON UNDERCOOING FOR COMMERCIAL Al-Si ALLOYS

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SLIDE 70

EFFECT OF Al-2Nb-2B ON COMMERCIAL Al-Si ALLOYS

The Charles Hatchett Award 2016 Lecture

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SLIDE 71

RESULTS

PISTON ALLOY (HYPER-EUTECTIC: 13 Wt.% Si)

740°C EFFECT OF Al-2Nb-2B ON COMMERCIAL Al-Si ALLOYS

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SLIDE 72

EFFECT OF Al-2Nb-2B ON COMMERCIAL Al-Si ALLOYS

The Charles Hatchett Award 2016 Lecture 740 oC

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SLIDE 73

EFFECT OF Al-2Nb-2B ON COMMERCIAL Al-Si ALLOYS

200 400 600 800 1000 1200 1400 1600 20 40 60 80 100

α-Al grain size [µm] Cooling rate, dT/dt [ C/s]

Al-7Si (Ref) Al-7Si (Al-2Nb-2B) Al-8.5Si (Ref) Al-8.5Si (Al-2Nb-2B) Al-10.5Si (Ref) Al-10.5Si (Al-2Nb-2B)

The Charles Hatchett Award 2016 Lecture

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SLIDE 74

Columnar grain structure

Chill zone

Fine (<0.5mm) equiaxed grains Al-10 Si alloy - Direct Chill Cast Billets

columnar Equiaxed Reference with Al-Nb-B

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SLIDE 75

Zone 4: equiaxed crystals Zone 3: long columnar crystals Zone 2: columnar crystals Zone 1: chilled zone Zone 1: chilled zone Zone 2: very fine equiaxed crystals Zone 3: fine equiaxed crystals

Reference Inoculated Nb-based compounds as heterogeneous nuclei

Al-10Si DC billets

The Charles Hatchett Award 2016 Lecture

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SLIDE 76

DC-SIMULATOR

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SLIDE 77

Comparative study between Al-Nb-B and Al-5Ti-B master alloys

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SLIDE 78

Al-2Nb-B master alloy addition

~ 300 µm Al-10Si ~ 4-5 mm

Al-5Ti-B master alloy addition

0.1%Ti 0.1% Nb

Comparison between Ti-B and Nb-B

The Charles Hatchett Award 2016 Lecture

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SLIDE 79

GRAIN REFINEMENT EFFICIENCY COMPARISON

WHEEL ALLOYS (HYPO-EUTECTIC: 7 Wt.% Si)

REFERENCE 0.1% Nb (AL-2Nb-2B) 0.1% Ti (Al-5Ti-1B) 0.2% MA (Al-5Ti-1B)

740°C

The Charles Hatchett Award 2016 Lecture

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SLIDE 80

Summary

  • Nb-B addition to Al-Si melt refines the grain structure of casting
  • End-user benefits:
  • Improved strength & ductility

 Lighter/thinner structures

  • Homogeneous properties (thick & thin sections)

 Complex structures

  • Tolerant to Fe contamination

 Closed loop recycling of scrap containing higher Fe

  • Reduced shrinkage porosity - Improved soundness

 Component rejection ratio can be minimised

The Charles Hatchett Award 2016 Lecture