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)?
 2011-0
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 200X Wecks
 2011-T3
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 200X Wecks
 3003
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 500X Wecks
 4032-T6
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 500X Wecks
 4147
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 500X Wecks
 5083-H321
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 500X Wecks
 6013-T8
Kellers (longitudinal) NaF-NaOH (transverse)

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 500X Wecks
 6061-T6511
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 200X Wecks
 6262-T9
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 200X Wecks
 7075-T651
Kellers NaF-NaOH

B&W
Bars are
20-m long
500X

Color is
Graff-Sargent 200X Wecks
 Alumec 89 (Al 2Cu 2.3Mg 6.3Zn 0.1Zr)

Kellers Reagent

Bars are 50 m, 200X