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Treatment of Micro Shrinkage in Ductile Iron with a FeSiLa Inoculant

Treatment of Micro Shrinkage in Ductile Iron with a FeSiLa Inoculant

Treatment of Micro Shrinkage in Ductile Iron with a FeSiLa Inoculant

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<strong>Treatment</strong> <strong>of</strong> <strong>Micro</strong><br />

<strong>Shr<strong>in</strong>kage</strong> <strong>in</strong> <strong>Ductile</strong> <strong>Iron</strong><br />

<strong>with</strong> a <strong>FeSiLa</strong> <strong>Inoculant</strong><br />

Steve Thelen<br />

Grede Biscoe<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


<strong>Shr<strong>in</strong>kage</strong> categories<br />

Suck Suck‐<strong>in</strong> <strong>in</strong><br />

0.2‐0.5 mm<br />

Macro<br />

<strong>Shr<strong>in</strong>kage</strong><br />

20 mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

<strong>Micro</strong><br />

<strong>Shr<strong>in</strong>kage</strong><br />

5 mm


<strong>Ductile</strong> <strong>Iron</strong> metallurgy: Solidification modes<br />

Temp °c<br />

1150 °C<br />

723 °C<br />

Hypoeutectic Hypereutectic<br />

L<br />

+<br />

Liquid<br />

L<br />

+<br />

Austénite Graphite<br />

Austenite + Graphite<br />

Ferrite e te + GGraphite ap te<br />

20 °C Ceq %<br />

3<br />

4<br />

5<br />

Fe – C Phase diagram (stable)<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

Eutectic Po<strong>in</strong>t


A<br />

Liquid<br />

<strong>Ductile</strong> <strong>Iron</strong> metallurgy: Hypereutectic mode<br />

Austenite<br />

+<br />

graphite<br />

1150°C<br />

Temp °c<br />

1150 °C<br />

L<br />

+<br />

Austénite<br />

D Austenite + Graphite<br />

Temp °C<br />

B, C<br />

A<br />

723 °C<br />

20 °C<br />

D<br />

3<br />

Ferrite + Graphite<br />

4<br />

B<br />

L<br />

+<br />

Graphite<br />

C<br />

5<br />

Ceq %<br />

<br />

T + dT<br />

timeDIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

Formation <strong>of</strong><br />

nuclei <strong>of</strong> primary<br />

graphite<br />

Grow<strong>in</strong>g <strong>of</strong> primary<br />

graphite <strong>in</strong> the<br />

liquid<br />

Formation Eutectic<br />

Austenite coated<br />

Graphite<br />

Progression <strong>of</strong> the<br />

Eutectic<br />

solidification<br />

& growth <strong>of</strong> graphite<br />

nodules


<strong>Shr<strong>in</strong>kage</strong> formation versus solidification<br />

Tempe rature<br />

LL+AA Liquid (L)<br />

L+ B<br />

Temp °C<br />

A+B Solidification <strong>of</strong><br />

compound A+B<br />

100% A 100% B<br />

% B <strong>in</strong> A<br />

Fe – C Phase diagram (stable)<br />

Liquid cool<strong>in</strong>g<br />

Typical <strong>Ductile</strong> <strong>Iron</strong> Thermal<br />

Analysis y curve<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

Formation and grow<strong>in</strong>g<br />

<strong>of</strong> B <strong>in</strong> the Liquid<br />

Solid cool<strong>in</strong>g<br />

Time


3<br />

Courtesy R. Hummer<br />

Cool<strong>in</strong>g and dilatation curves<br />

2<br />

1<br />

0.2‐0.5 mm<br />

Temp °C<br />

1150°C 1150 C<br />

1 2 3<br />

20mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

5 mm<br />

time


<strong>Micro</strong> shr<strong>in</strong>kage<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


“La” La mechanisms to elim<strong>in</strong>ate <strong>Micro</strong> <strong>Shr<strong>in</strong>kage</strong><br />

• These works have been done <strong>in</strong> collaboration <strong>with</strong>:<br />

IRC University <strong>of</strong> Birm<strong>in</strong>gham (United K<strong>in</strong>gdom)<br />

R A Hard<strong>in</strong>g Hard<strong>in</strong>g, J Campbell<br />

Pech<strong>in</strong>ey’s Pech<strong>in</strong>ey s Research Central Laboratory (France)<br />

T Margaria<br />

&<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Lanthanum effect is well known…<br />

• History:<br />

- US Patent 2.970.902 – Alexander & Spengler – 1956<br />

- Improved mach<strong>in</strong>ability<br />

- EP Patent 4819 – Gorger<strong>in</strong>o - 1978<br />

- FR Patent 024855 – 1979<br />

- La efficient element to counter <strong>Micro</strong> <strong>Shr<strong>in</strong>kage</strong><br />

“La” bear<strong>in</strong>g g MgFeSi g : In-Mold process p = success<br />

• “La” bear<strong>in</strong>g MgFeSi : Ladle process = low repeatability due<br />

to the difficulty <strong>in</strong> an <strong>in</strong>dustrial environment <strong>of</strong> ma<strong>in</strong>ta<strong>in</strong><strong>in</strong>g<br />

the adequate and repeatable amount <strong>of</strong> La content <strong>in</strong> order<br />

to exercise on the molten metal the desired effects. Rapid<br />

fade as La fades quicker q than Mg g <strong>in</strong> molten iron.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Stages g <strong>of</strong> Solidification<br />

• Columnar Solidification<br />

– First solids appear on the mold walls, walls<br />

near locations <strong>of</strong> severe heat loss.<br />

Gra<strong>in</strong>s grow <strong>in</strong> the opposite direction <strong>of</strong><br />

hheat t flow, fl usually ll perpendicular di l to t the th<br />

mold walls.<br />

• Equiaxed Solidification<br />

– After heat flow through the walls is<br />

reduced, particles <strong>of</strong> the columnar<br />

gra<strong>in</strong>s detach and grow freely <strong>in</strong> the<br />

liquid. “Equally” on every “axis”.


Solidification mode:<br />

• Stages <strong>of</strong> solidification <strong>in</strong> a mold<br />

– Columnar, perpendicular to mold walls, opposite to the direction <strong>of</strong> heat flow.<br />

– Equiaxed, When the heat flow reduced, particles from columnar zone detach and<br />

grow freely.<br />

Columnar zone Equiaxe solidification<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Solidification mode: Influenc<strong>in</strong>g factors<br />

Influenc<strong>in</strong>g factors:<br />

High nucleation favors the Equiaxe mode by<br />

develop<strong>in</strong>g more solidification sites <strong>in</strong> the liquid.<br />

Stirr<strong>in</strong>g motions favors the Equiaxe mode<br />

Other phenomena affect the transition between the<br />

columnar to Equiaxe mode<br />

heat flow<br />

nature nature <strong>of</strong> solute elements at the solidification <strong>in</strong>terface<br />

(segregation , …)<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Experiments<br />

• Pr<strong>in</strong>ciple<br />

– Measurements <strong>of</strong> the columnar zone thickness at<br />

given solidification times & “La” addition rates, to<br />

demonstrate the effect <strong>of</strong> “La” on an iron<br />

solidification growth process.<br />

– 0.15% addition <strong>of</strong> a late stream <strong>in</strong>oculant.<br />

– La amount <strong>in</strong> the <strong>in</strong>oculant varied from 0% to 2,4%.<br />

– <strong>Treatment</strong>s are poured at the same temperature<br />

<strong>in</strong>to a mold.<br />

– At a given g time and targeted g 50% liquid/solid q ratio<br />

the molds are emptied <strong>of</strong> their rema<strong>in</strong><strong>in</strong>g semi<br />

solid iron.<br />

– The solidified iron shell thickness was measured. measured<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Experimental procedure<br />

Melt<strong>in</strong>g<br />

<strong>FeSiLa</strong><br />

<strong>Treatment</strong> and pour<strong>in</strong>g <strong>in</strong> the mold Solidification<br />

Thickness<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

Empty<strong>in</strong>g


Experimental p pprocedure:<br />

Results<br />

• On 60 mm diameter molds (IRC):<br />

% La <strong>in</strong> <strong>Inoculant</strong> Thickness<br />

0% 6 mm<br />

0,8% 2 mm<br />

24% 2,4% 05mm 0,5 mm<br />

On On 100 mm diameter molds (LCR):<br />

% La <strong>in</strong> <strong>Inoculant</strong> Thickness<br />

0% 8mm 8 mm<br />

0,8% 2 mm<br />

2,4% 1,1 mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Experimental procedure: Results<br />

Without La 0%<br />

Diameter 60 mm<br />

Thickness 6 mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Experimental procedure: Results<br />

With La 0.8%<br />

Diameter 60 mm<br />

Thickness 2 mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Experimental p pprocedure:<br />

Results<br />

Without La 0%<br />

With La 0.8%<br />

Diameter 60 mm Diameter 60 mm<br />

Thickness 6 mm Thickness 2 mm<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Lanthanum effect on solidification<br />

• Lanthanum promotes p the equiaxe q<br />

solidification mode by:<br />

Develop<strong>in</strong>g p g a higher g nucleation power, p , therefore more<br />

solidification sites are <strong>with</strong><strong>in</strong> the molten iron.<br />

Modify<strong>in</strong>g the molten iron viscosity viscosity, favor<strong>in</strong>g stirr<strong>in</strong>g motions<br />

<strong>with</strong><strong>in</strong> the molten iron.<br />

Restrict<strong>in</strong>g the growth <strong>of</strong> columnar gra<strong>in</strong>s.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Consequences q for <strong>Micro</strong> <strong>Shr<strong>in</strong>kage</strong> g<br />

• At a given solidification stage, when “La” is added, the equiaxe<br />

solidification is favored:<br />

– Thickness <strong>of</strong> the columnar zone is reduced: a larger volume <strong>of</strong><br />

free flow<strong>in</strong>g liquid is created allow<strong>in</strong>g molten iron to travel<br />

<strong>with</strong><strong>in</strong> channels thus aid<strong>in</strong>g the feed<strong>in</strong>g <strong>of</strong> the cast<strong>in</strong>g. cast<strong>in</strong>g<br />

– Semi-solid iron conta<strong>in</strong>s more solid particles after fill<strong>in</strong>g <strong>of</strong> a<br />

given volume chamber : less liquid is needed to compensate<br />

the solidification contraction.<br />

– PPromotion i <strong>of</strong> f Late eutectic i graphite hi precipitation. i i i<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Industrial examples: Crankshafts<br />

Without La<br />

With La<br />

• Th The use <strong>of</strong> f <strong>FeSiLa</strong> F SiL allow: ll <strong>Micro</strong>structure Mi t t – CCast<strong>in</strong>gs ti per mold ld<br />

Courtesy Française de Mécanique<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


US Trials, The Cast<strong>in</strong>g<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The Cast<strong>in</strong>g<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The Problem<br />

• An 11 pound crankshaft adapter.<br />

• Orig<strong>in</strong>ally ran >10% for shr<strong>in</strong>kage. shr<strong>in</strong>kage<br />

• Gat<strong>in</strong>g changes brought shr<strong>in</strong>kage<br />

down to about 3% at level 3. 3<br />

• Inoculation practice, 5 pounds per<br />

tton <strong>of</strong> f 75% FFoundry d GGrade d<br />

Ferrosilicon.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The Solution<br />

• Ma<strong>in</strong>ta<strong>in</strong> current gat<strong>in</strong>g system.<br />

• Remove 5 pounds per ton <strong>of</strong> 75% Foundry<br />

Grade Ferrosilicon <strong>in</strong>oculant.<br />

• Add 5 pounds per ton <strong>of</strong> <strong>FeSiLa</strong> <strong>in</strong>oculant.<br />

– Silicon 45 to 50%<br />

– Calcium 1.50 to 2.50 %<br />

– Alum<strong>in</strong>um 1.25% maximum<br />

– Lanthanum 1.80 to 2.20%<br />

– This is a 0.005% 0 005% La addition addition.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The First Test<br />

Tightened acceptable shr<strong>in</strong>kage from level 3<br />

down to level 2.<br />

Ran 138 pieces <strong>with</strong> <strong>FeSiLa</strong> alloy <strong>in</strong>oculant. <strong>in</strong>oculant<br />

The 138 pieces were captured and placed <strong>in</strong>to 1<br />

b<strong>in</strong>.<br />

Ran 333 pieces <strong>with</strong> Foundry Grade <strong>in</strong>oculant.<br />

The 333 pieces were captured and placed <strong>in</strong>to 2<br />

bi b<strong>in</strong>s.<br />

122 pieces <strong>in</strong> b<strong>in</strong> # 2.<br />

211 pieces <strong>in</strong> b<strong>in</strong> # 3.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The Results<br />

B<strong>in</strong> # 1, <strong>with</strong> <strong>FeSiLa</strong> <strong>in</strong>oculant ran shr<strong>in</strong>kage<br />

ffree <strong>with</strong> i h 138 out <strong>of</strong> f 138 pieces i show<strong>in</strong>g h i no llevel l<br />

<strong>of</strong> shr<strong>in</strong>kage.<br />

B<strong>in</strong> #2, <strong>with</strong> Foundry Grade FeSi <strong>in</strong>oculant.<br />

122 total pieces, 10 pieces <strong>with</strong> shr<strong>in</strong>kage<br />

4 pieces level 2, accepted<br />

6 pieces level 3 or higher, rejected<br />

B<strong>in</strong> # 3, <strong>with</strong> Foundry Grade FeSi <strong>in</strong>oculant.<br />

211 total pieces, 10 pieces <strong>with</strong> shr<strong>in</strong>kage<br />

4 pieces level 2 or less, accepted<br />

6 pieces level 3 or higher, rejected.<br />

12 pieces scrapped from 333 pieces <strong>in</strong> B<strong>in</strong>s #2<br />

and 3 for a scrap rate <strong>of</strong> 3.60%.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


250<br />

200<br />

150<br />

100<br />

50<br />

0<br />

First Test Test, B<strong>in</strong> Results<br />

138<br />

0<br />

0<br />

211<br />

122 Pieces<br />

10 10<br />

6 6<br />

B<strong>in</strong> 1 <strong>FeSiLa</strong> B<strong>in</strong> 2 FeSi B<strong>in</strong> 3 FeSi<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

Shr<strong>in</strong>k, Total<br />

Shr<strong>in</strong>k Shr<strong>in</strong>k, Rejectable


9<br />

8<br />

7<br />

6<br />

5<br />

4<br />

3<br />

2<br />

1<br />

0<br />

First test, shr<strong>in</strong>kage g<br />

breakdown<br />

0 0<br />

8.2<br />

4.92<br />

B<strong>in</strong> 1 <strong>FeSiLa</strong> B<strong>in</strong> 2 FeSi B<strong>in</strong> 3 FeSi<br />

4.74<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

2.84<br />

% Shr<strong>in</strong>k<br />

% Reject


The Mistake<br />

• The foundry mistakenly reverted back<br />

to the orig<strong>in</strong>al practice, practice mak<strong>in</strong>g anther<br />

1,455 pieces, 6 b<strong>in</strong>s, <strong>with</strong>out the <strong>FeSiLa</strong><br />

<strong>in</strong>oculant.<br />

• The choice was to either scrap the<br />

entire run, or 100% <strong>in</strong>spect by x-ray<br />

sort sort. They decided to 100% <strong>in</strong>spect. <strong>in</strong>spect<br />

• Of the 1,455 pieces, 37 were rejected<br />

and 1,419 , were acceptable p for a 2.54%<br />

scrap rate.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


The Results from the<br />

Mistake<br />

• All b<strong>in</strong>s had Foundry Grade 75% FeSi <strong>in</strong>oculant.<br />

– B<strong>in</strong> # 1 had 231 pieces.<br />

• 5 pieces <strong>with</strong> level 3 shr<strong>in</strong>kage, rejected.<br />

– B<strong>in</strong> # 2 had 234 pieces.<br />

• 10 pieces <strong>with</strong> level 3 or higher shr<strong>in</strong>kage, rejected.<br />

– B<strong>in</strong> # 3 had 271 pieces.<br />

• 3 pieces <strong>with</strong> level 3 shr<strong>in</strong>kage, rejected.<br />

– Bi B<strong>in</strong> # #4h 4 had d259 259 pieces. i<br />

• 6 pieces <strong>with</strong> level 3 shr<strong>in</strong>kage, rejected.<br />

– B<strong>in</strong> # 5 had 263 pieces.<br />

• 10 pieces <strong>with</strong> level 3 shr<strong>in</strong>kage, shr<strong>in</strong>kage rejected rejected.<br />

– B<strong>in</strong> # 6 had 197 pieces.<br />

• 3 pieces had level 3 shr<strong>in</strong>kage, rejected.<br />

– Overall scrap rate 22.54% 54%<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


300<br />

250<br />

200<br />

150<br />

100<br />

50<br />

0<br />

Second Run, B<strong>in</strong> Results<br />

231<br />

5<br />

234<br />

10<br />

271<br />

259<br />

3 6<br />

263<br />

197<br />

B<strong>in</strong> 1 FeSi B<strong>in</strong> 2 FeSi B<strong>in</strong> 3 FeSi B<strong>in</strong> 4 FeSi B<strong>in</strong> 5 FeSi B<strong>in</strong> 6 FeSi<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

10<br />

3<br />

Pieces<br />

Shr<strong>in</strong>k, Total<br />

Shr<strong>in</strong>k, Rejectable


Second Run, <strong>Shr<strong>in</strong>kage</strong><br />

4.5 4.27<br />

4<br />

3.5<br />

3<br />

2.5<br />

2<br />

1.5<br />

11<br />

0.5<br />

0<br />

2.16<br />

Results<br />

1.11<br />

B<strong>in</strong> 1 FeSi B<strong>in</strong> 2 FeSi B<strong>in</strong> 3 FeSi B<strong>in</strong> 4 FeSi B<strong>in</strong> 5 FeSi B<strong>in</strong> 6 FeSi<br />

2.32<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011<br />

3.8<br />

1.52<br />

% Shr<strong>in</strong>k<br />

% Reject


The End<strong>in</strong>g<br />

The The foundry did not conduct another “Trial Trial<br />

<strong>with</strong> the <strong>FeSiLa</strong> <strong>in</strong>oculant” due to the cost<br />

<strong>of</strong> 100% x-ray <strong>in</strong>spection <strong>of</strong> the 1,455<br />

pieces pieces.<br />

S<strong>in</strong>ce that time, the foundry has shipped<br />

over 9,000 pieces to their customer while<br />

us<strong>in</strong>g i the th <strong>FeSiLa</strong> F SiL <strong>in</strong>oculant. i l t<br />

The foundry has not had a s<strong>in</strong>gle compla<strong>in</strong>t<br />

for porosity p y s<strong>in</strong>ce the implementation p<br />

<strong>of</strong> the<br />

<strong>FeSiLa</strong> <strong>in</strong>oculant as standard practice for<br />

this part.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Thank You<br />

• The presenter would like to<br />

acknowledge and thank:<br />

– R Siclari, T Margaria, E Bethelet and J<br />

Fourmann for their paper p p titled “<strong>Micro</strong>-<br />

shr<strong>in</strong>kage <strong>in</strong> <strong>Ductile</strong> <strong>Iron</strong> / Mechanism &<br />

Solution” which was orig<strong>in</strong>ally<br />

presented at the 2003 Keith Millis<br />

Symposium on <strong>Ductile</strong> Cast <strong>Iron</strong>.<br />

– Jim Csonka, Hickman, Williams &<br />

Company for the technical assistance <strong>in</strong><br />

prepar<strong>in</strong>g this presentation.<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011


Questions?<br />

DIS DIS Annual Annual Meet<strong>in</strong>g, Meet<strong>in</strong>g, June June 2, 2, 2011 2011

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