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Metallographic Etching of Aluminum and Its Alloys

George F. Vander Voort Buehler Ltd. Lake Bluff, Illinois USA And Elena P. Manilova Polzunov Institute St. Petersburg, Russia

Preparation of Aluminum Specimens


Grind with 240-grit SiC water-cooled paper, 240 rpm, 5 lbs. (20N) per specimen, until co-planar Polish with 9-m Diamond on an Ultra-Pol (silk) cloth, 150 rpm, 5 lbs/specimen, 5 minutes (contra rotation) Polish with 3-m Diamond on a Trident cloth, 150 rpm, 5 lbs/specimen, 4 minutes (contra rotation) Polish with 1-m Diamond on a Trident cloth, 150 rpm, 5 lbs/specimen, 3 minutes (contra rotation) Polish with 0.05-m Colloidal Silica on a Microcloth pad, 120 rpm, 5 lbs/specimen, 3 minutes (contra rotation) (Contra: Head and platen rotate in opposite directions)

Standard Black&White Etchants for Aluminum


Kellers Reagent 95 mL water, 2.5 mL HNO3, 1.5 mL HCl, 1.0 mL HF Immerse Caustic Sodium Fluoride Etch 93 mL water, 2 g NaOH, 5 g NaF Graff-Sargent Etch 84 mL water, 15.5 mL HNO3, 0.5 mL HF, 3 g CrO3

Anodizing with Barkers Reagent


1.8% Fluoboric acid in water 20-45 V dc, for up to 2 minutes Examine with crossed polarized light, plus a sensitive tint (first order red plate, or plate) to see the microstructure in color. It is good for grain size, but does not reveal alloy segregation.

Examples of Anodizing with Barkers Reagent


It does not reveal alloy segregation in cast alloys but does display the dendrites well. It is widely applicable for revealing grain structure in wrought alloys But, you must have a conductive path.

Bright Field

Polarized Light

PL + Sensitive Tint

100 m

100 m

Grain structure of wrought 1100 grade foil after electrolytic polishing and anodizing with Barkers reagent (20 V dc, 2 min), and viewed with bright field (top), polarized light (left) and with polarized light plus a sensitive tint filter (right). Note that color is not observed in bright field because an interference film is not formed using Barkers reagent.

As-cast (concast) 1100 Al (>99% Al) anodized with Barkers reagent (30 V dc, 2 min.) revealed a dendritic solidification structure. Note that no evidence of segregation is apparent. Original at 50X. Viewed with crossed polars + sensitive tint.

Wrought 2024-F aluminum (Al 4.4% Cu 1.5% Mg 0.6% Mn) bar (28.5 mm diam.) showing the grain structure and intermetallics. Magnification bar is 200 m long. Anodized with Barkers reagent (30 V dc, 2 min.). Transverse plane.

Wrought 5754-F aluminum strip (Al 3.2% Mg 0.4% Mn + Cr) anodized with Barkers reagent (30 V dc, 2 min.). The strip was cold worked and annealed at 343 C (650 F) for 2 h. The grain structure is fully recrystallized.

Wrought 6005 aluminum (Al 0.5% Mg 0.8% Si) anodized with Barkers reagent (20 V dc, 2 min.) revealing an equiaxed alpha grain structure. Original at 50X. Viewed with crossed polarized light plus sensitive tint.

Sheared end of 6061-F (Al 1% Mg 0.6% Si 0.2% Cr 0.27% Cu) extruded rod anodized with Barkers reagent (30 V dc, 2 min.) revealing the heavily elongated grains from extruding and the compression of the sheared end. Magnification bar is 100 m long.

Wrought 7075-T74 aluminum (Al 1.6% Cu 2.5% Mg 5.6% Zn 0.23% Cr) anodized with Barkers reagent (20 V dc, 2 min.) showing highly elongated, recrystallized surface grains on a fine grained interior structure. Magnification bar is 50 m long. Viewed with crossed polarized light plus sensitive tint.

Color Tint Etching With Wecks Reagent


100 mL water 4 g KMnO4 1 g NaOH Use at room temperature Immerse up to 20 s, or longer, until surface is colored

Examples of the Use of Wecks Reagent


Easier to obtain good results with castings compared to wrought grades. Easy to mix and use, not particularly dangerous. Reveals segregation very well. Grain structure can be revealed with most wrought compositions

As-cast (concast) 3004 aluminum (Al 1.25% Mn 1.05% Mg) tint etched with Wecks reagent and viewed with crossed polars plus sensitive tint. Magnification bar is 50 m long. Reveals segregation (coring) within the dendrites and intermetallics between the dendrites.

As-cast 206 aluminum (Al 4.4% Cu 0.3% Mg 0.3% Mn) tint etched with Wecks reagent and viewed with crossed polars + sensitive tint. Magnification bar is 50 m long.

As-cast 319 aluminum (Al 6.0% Si 3.5% Cu) tint etched with Wecks reagent and viewed with crossed polarized light. Magnification bar is 100 m long.

As-cast 319 aluminum (Al 6.0% Si 3.5% Cu) tint etched with Wecks reagent and viewed with crossed polarized light. Magnification bar is 100 m long.

As-cast (concast) 1100 Al (>99% Al) tint etched with Wecks reagent revealing a dendritic solidification structure. Note that the segregation is revealed vividly. Magnification bar is 200 m long. Viewed with crossed polars + sensitive tint.

Cast A356 Aluminum

Small Permanent Mold Casting, 200X

Large Permanent Mold Casting, 200X

Dendritic structure and eutectic structure of A356 permanent mold castings revealed using Wecks reagent (polarized light plus sensitive tint, 200X)

Cast A356 Aluminum

Thixocast, 200X

Thixocast and Thixoformed

Microstructure of A356 made by thixocasting and by thixocasting and thixoforming revealed using Wecks reagent (viewed with polarized light and sensitive tint, 200X).

Cast A356 VRC/PRC

Cast structure of VRC/PRC cast A356 aluminum revealed using Wecks reagent (polarized light plus sensitive tint, 200X)

Microstructure of an SSM billet of A357 aluminum etched with Wecks and viewed in bright field (200x).

Dendrites of -Al and a eutectic of -Al and Si in as-cast Al 7.12% Si etched with Wecks, polarized light plus sensitive tint.

Near-eutectic microstructure of as-cast Al 11.7% Si alloy etched with Wecks and viewed with polarized light plus sensitive tint.

Hypereutectic as-cast Al 19.85% Si with proeutectic Si and a eutectic of -Al and Si etched with Wecks and viewed with polarized light plus sensitive tint.

As-Cast Al Cu Alloys
Al 33% Cu Al 45% Cu

Eutectic in the Al-Cu system at 33% Cu is shown at left at 1000X. The AlCu2 phase was colored red using 1 g ammonium molybdate, 6 g ammonium chloride and 200 mL water. Hypereutectic Al 45% Cu is shown at right at 50X. The AlCu2 was colored blue using 1 part 3g ammonium molybdate, 20 mL HNO3, 20 mL water to 4 parts ethanol.

Surface

Interior

Microstructure of pressure-die cast A380 aluminum (Al 8.5% Si 3.5% Cu) etched with Wecks reagent and photographed in bright field illumination. Note that the silicon particles were colored by the reagent. The magnification bars are both 50 m long.

Poor Preparation Yields Bad Results!

Example of poor etch results with Wecks when a specimen of 2519 plate was improperly prepared (polarized light plus sensitive tint).

Aluminum Clad 2024 Aluminum

Wecks Reagent

Kellers/Wecks Reagents

Microstructure of Al-clad 2024 aluminum etched with Wecks tint etch (left) and with Kellers reagent followed by Wecks (right). Wecks reagent reveals the interface much better than standard reagents. Kellers reveals the grain structure. The magnification bars are both 50 m long.

Weld

Base

Microstructure of a friction stir weld in 2519 aluminum (Al 5.8% Cu 0.3% Mn 0.3% Mg 0.06% Ti 0.1% V 0.15% Zr) etched with Wecks reagent and viewed with polarized light plus sensitive tint. Original at 100X. The magnification bar is 100 m long.

left side

right side

Very fine grain structure in the weld zone of the 5083-H321 friction stir weld, etched with Wecks and viewed with polarized light and sensitive tint.

Friction Stir Weld in 7075-T651

Wecks reagent used to reveal a friction stir weld in 7075-T651. The magnification bar is 200 m long.

Al Al2O3 composite etched with Wecks and viewed with polarized light plus sensitive tint.

Al Al2O3 composite etched with Wecks and viewed with polarized light plus sensitive tint.

7075 aluminum containing hollow ceramic spheres, etched with Wecks and viewed with polarized light and sensitive tint.

Laser Weld Nugget - 6061

Base

Heat Affected Zones


Microstructure of a laser weld in 6061 aluminum (Al 0.6% Si 0.3% Cu 1% Mg 0.2% Cr) etched with Wecks reagent and viewed with polarized light plus sensitive tint. Original at 50X. The magnification bar is 200 m long.

Grain Size Etching Experiments

Compare results from etching with Kellers, caustic sodium fluoride, Graff-Sargent and Wecks reagents using common wrought aluminium alloys. What can we do to reveal grain boundaries without going to electrolytic anodizing with Barkers reagent (or a similar formulation)?

Kellers

2011-0

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 200X Wecks

Kellers

2011-T3

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 200X Wecks

Kellers

3003

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 500X Wecks

Kellers

4032-T6

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 500X Wecks

Kellers

4147

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 500X Wecks

Kellers

5083-H321

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 500X Wecks

Kellers (longitudinal)

6013-T8

NaF-NaOH (transverse)

B&W Bars are 20-m long 500X Graff-Sargent Color is 500X Wecks

Kellers

6061-T6511

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 200X Wecks

Kellers

6262-T9

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 200X Wecks

Kellers

7075-T651

NaF-NaOH

B&W Bars are 20-m long 500X Graff-Sargent Color is 200X Wecks

Alumec 89 (Al 2Cu 2.3Mg 6.3Zn 0.1Zr)


Kellers Reagent

Bars are 50 m, 200X