Metallographic preparation of

aluminium and aluminium alloys

Application
Unlike other long established metals such
as iron and copper, aluminium is a relatively
Notes
young metal and has been known only since
the beginning of the 19th century. In 1886 a
production method for aluminium was
developed which is still used today:
the Hall-Heroult-Process.

Aluminium has a silvery white appearance,

is very light and is used as pure metal or
alloyed for a multitude of different applica-
tions. Only very small amounts of alloying
elements can increase the strength, and due
to their low density, aluminium alloys are
especially suited for applications in the air-
Aluminium-silicon cast, colour etched with
craft and aerospace industry. Also aluminium molybdic acid, 200x.
alloys are used frequently in the automobile
industry to promote weight reductions. New alloys such as Al-Li and Ti-Al are manu-
factured by powder metallurgical process
The high corrosion resistance of aluminium and aluminium is also used as matrix metal
is based on a passive film of aluminium for composites. Being a very multifaceted
oxide that is intimately connected to the material, aluminium will in future open up
surface. This oxide film is capable of renew- more fields for new applications.
ing itself spontaneously when the surface is
damaged. Therefore aluminium is suited for Metallography of aluminium is used in qual-
polished and brushed surfaces and for an- ity control for grain size determination and
odising in various colours, which makes it an for micro structure defects on the polished
interesting material for the building industry. and etched specimen. In addition, the sam-
ple is checked for impurities such as oxides
Additional properties of aluminium are its or zirconium aluminides (Fig. 2). Cast mate-
high heat conductivity and its easy form- rial is evaluated for shape and distribution
ability, either by casting, hot or cold working of phases and possible porosity. In wrought
or machining. Aluminium is non-toxic and material, defects from the rolling and extru-
neutral regarding taste and is therefore the sion process are investigated and plating
preferred material for the food and packaging thicknesses measured.
industry, for instance for cans and foils or
machines for bakeries and beverage pumps.

Difficulties during metallographic preparation Solution

- Pure aluminium is very soft and prone to - Severely worked and deformed wrought - Plane grinding with the finest possible
mechanical deformation and scratching. alloys are difficult to contrast SiC-Foil/Paper
- Silicon carbide and diamond particles can - Diamond polishing and/or final polishing
be pressed into the specimen surface (Fig.1) need to be long enough to remove all
embedded particles
- Final polishing with Collodial Silica
suspension
- Anodising with Barker’s reagent

Fig.1: Embedded diamond particles in pure aluminium Fig. 2: Oxide in the surface of an aluminium pressure
after polishing with 3 µm, 200x. die casting, 50x.
Production and Bauxite

application of Alumina Extraction Scrap

aluminium Alumina Pure Mixed

Hall-Heroult Process Secondary Melting

Primary Aluminium Secondary Aluminium

Alloy amount Alloy amount
approx. 2% < 15%
Aluminium is one of the most frequently
occuring metals in the earth’s crust. It is not
found in its pure state but combined in the Rolling Mill Foundry Scrap
form of chemical compounds. An economi-
cal extraction is only possible from bauxite Semi-finished Products Casts
which consists of 60% aluminium oxide as
hydroxide (Al2O3 + H2O), the rest are metal
oxides (Fe203, Si02, Ti02). The production FINAL PRODUCTS Scrap
process is complex and energy intensive and
is mainly based on two steps that are briefly
Consumer Scrap Simplified diagram of
described in the following. the aluminium
production process.
Extraction of pure alumina
(aluminium oxide, Al2O3) from bauxite
Alumina recovery begins by crushing and
finely grinding the bauxite and heating it
with sodium hydroxide under pressure. In Alumina Graphite anodes
this process a water soluble sodium alumi- Cryolite
nate is formed together with undissolved
Alumina crust CO + CO2
residues of iron, titanium and silicon, called
5 Volt
“red mud” that is separated by sedimenta- 150 kA
tion. To the highly diluted sodium aluminate Electrolyte/Melt
solution “seed crystals” of fresh aluminium
hydroxide are added to initiate the precipita- Molten aluminium

tion of pure aluminium hydroxide (Al(OH)3). Carbon cathode

Through calcination at 1200°C the water Al Busbar
is removed from aluminium hydroxide and
pure anhydrous alumina (aluminium oxide)
remains.
Schematic drawing of the
electrolysis producing
The Hall-Heroult process: pure aluminium.
Converting alumina to aluminium
The reaction chemistry of pure alumina
requires an electro-chemical process to The molten aluminium has a higher density The diagram shows the cycle of aluminium
extract aluminium from its oxide. As the than the electrolyte-melt and settles at the with its production steps. The main products
melting point of aluminium oxide is very bottom of the pot. It is tapped once a day are wrought alloys for semi-finished products
high, 2050°C, it is mixed with cryolite which and cast into pigs. With this process, alu- containing up to 2% alloying elements and
reduces the melting point to 950°C. In addi- minium of 99.0 – 99.9% purity is produced cast alloys with up to 15% alloying elements.
tion, the cryolite increases the conductivity of which the largest part is used for the
and consequently the electricity yield. production of aluminium alloys. There are numerous aluminium alloys and
they are categorised as wrought and cast
The electrolysis takes place in a large carbon Through an additional electrolysis the alloys. These two groups are differentiated
or graphite lined steel container that con- purity of the aluminium can be increased to again by heat-treatable and non-heat-
tains steel rods for conducting electricity. 99.98% for semi-finished products and to treatable alloys. The addition of very small
The carbon clad walls and floor form the 99.99% for pig casts. This pure aluminium amounts of alloying elements produce an
cathode and the aluminium oxide-cryolite has a very high corrosion resistance and is increase in tensile strength, yield strength
melt is the electrolyte. Carbon blocks hang particularly well suited for anodising. It is and hardness when compared with the
on a rack over the melt function as anodes. used for brightening products such as deco- mechanical properties of pure aluminium.
During the electrolysis the carbon of the rative trim, reflectors, foils for electrolyte- The most important alloying elements are Si,
anode reacts with the oxygen of the alumina capacitors and for tubes in the chemical Mg, Cu, Zn and Mn. Combinations of alloying
and in a secondary reaction, metallic alu- and food industry. As the cost of aluminium elements with aluminium or with each other
minium is produced with the formation of increases with increasing purity, the purity (Mg2Si, Al2Cu, MgZn2 and Al-Fe-Si
carbon dioxide: of a specific aluminium used for a product compounds) influence the workability. These
is determined by the requirements of its mostly eutectic compounds have to be finely
2 Al2O3 + 3 C → 4 Al + 3 CO2 application. dispersed first through a hot working process
before the alloy can be cold worked.
Lamps with reflectors of highly ing. Only after this hot forming, in which the Plated sheet, core: aluminium alloy 3503, plating:
polished aluminium. aluminium alloy 4104, unetched 100x.
embrittling eutectic grain and cell boundary
structure is broken up, is the cold working of
The most important process to improve the wrought alloys possible (Fig. 3-5).
mechanical properties of aluminium alloys The main alloying elements for wrought alu-
is age hardening. It requires a solid solution minium alloys are copper, magnesium, zink
with a decreasing solubility of the alloying and manganese. Silicon and iron affect the
elements with falling temperatures, for ins- mechanical properties and corrosion resis-
tance AlCuMg and AlMgSi. tance and can either be impurities or alloying
elements, depending on the requested purity
Natural age hardening (example AlCuMg). and application.
After solution annealing the workpiece is
quenched and consequently the precipitation Wrought alloys are for example used for
of the Al2Cu in the solid solution is sup- plates in mechanical engineering and mould Plated sheet, core: aluminium alloy 2024, plating:
pressed. The workpiece is then left to age in construction, for rolled products such as aluminium 99.5%, etched with Dix and Keller, 50x.
ambient temperature. During this process sheet and strip and for plated products like
the aluminium lattice precipitates the cop- radiators and heat exchangers. Plated sheets High strength aluminium wrought alloys are
per from the supersaturated solution. The which have to combine specific mechanical used in mechanical engineering, conveying
resultant strain produced in the aluminium properties and high corrosion resistance and electro technical applications and for
lattice leads to an increase in strength and have a core billet of an aluminium alloy that sports and leisure products such as bind-
hardness. Natural hardening takes approx. is covered on both sides with pure aluminium ings for snowboards, ski poles and gears for
5-8 days. and rolled. These plated sheets are used for mountain bikes etc.
specific semi-finished products for aircraft Aluminium is increasingly used as matrix
In the artificial age hardening process the construction or for decorative applications material for composites, especially for fibre
dynamics are the same as described above. such as trim and reflectors. reinforced aluminium in the aircraft and
However, ageing takes place at an elevated aerospace industries.
temperature. For instance, for an AlMgSi al-
loy, ageing occurs in 4-48 hrs at 120-175°C
after solution annealing and quenching.
The precipitation of the Mg2Si phase pro- Non hardening alloys are work hardened through cold working

duces internal strain in the aluminium lattice Main alloying element Serial number Examples of alloys
which results in an increase of strength and
More than 99% pure, with traces of Cu, Fe, Si 1xxx Al 99,0; Al 99,5; Al 99,85
hardness.
Mn 3xxx Al-Mn; Al-Cu-Mn-Mg

Wrought alloys Mg 5xxx AlMg3; Al-Mg-Mn-Cr

Billets for rolling and ingots for pressing are Other elements 8xxx Al-Fe-Si; Al-Li-Mg-Cu
produced in a continuous casting process. Hardening alloys are hardened through natural and artificial hardening
In many cases casting is followed by anneal-
ing for homogenisation. Transformation of Cu 2xxx Al-Cu-Si-Mg

the cast structure into a wrought structure Si 4xxx Al-Si-Mg

is effected by hot rolling, extrusion or forg- Mg, Si 6xxx Al-Mg-Si
Zn 7xxx Al-Zn-Mg-Cu

Fig. 3: Aluminium alloy 2024, cast, showing eutectic Fig. 4: As Fig. 3, homogenised, unetched, 200x. Fig. 5: As Fig. 4, hot rolled, unetched, 200x.
precipitation on grain boundaries, unetched, 200x.
 ß-AlFeSiMn Difficulties during Recommendations
α-AlFeSiMn
Al2Cu
the preparation for the preparation
of aluminium and of aluminium and
Si
aluminium alloys aluminium alloys

Fig. 6: AlSi6Cu4 cast, the various phases can be With increasing purity, aluminium becomes For sectioning of aluminium a hard silicon
identified by there typical colour.
softer and more susceptible to mechanical carbide cut-off wheel is used that is
deformation and scratches. Consequently, generally suitable for non-ferrous metals.
Cast alloys grinding can cause already deep deformation For mounting resin a phenolic resin is in
Aluminium casts are mainly alloyed to im- in high purity aluminium. most cases sufficient. Thin sheets and
prove the mechanical properties and are dif- Grinding and polishing abrasives can be foils and specimens for anodising are best
ferentiated according to their main alloying pressed into the surface. With increasing mounted in slow curing epoxy resins,
elements silicon, magnesium and copper. alloying content aluminium becomes harder whereby the samples should protrude from
Alloy contents that exceed the saturation of and cast alloys are relatively easy to prepare. the back of the mount to serve as electrical
the solid solution are precipitated as pure It needs to be emphasised though, that the contacts.
metal such as silicon or as eutectics and aluminium matrix has to be well polished in
inter metallic phases. order to avoid errors in the structure inter- Mechanical grinding and polishing
pretation (Fig. 9 and 10). It is recommended that plane grinding is
Silicon increases the castability of alumini- carried out with the finest possible grit in
um, and in eutectic alloys, such as AlSi12, order to avoid any excessive mechanical
small amounts of sodium are added before deformation. Hardness, size and number of
casting to refine the eutectic. In this refining samples have to be taken into account, but
process, instead of precipitating as coarse even with larger samples of pure aluminium,
needles or plates (Fig. 7), silicon forms a 500# is sufficient for plane grinding. Large
very fine eutectic with the α-solid solution cast parts of aluminium alloys can be
(Fig. 8). The effect of hardening in these al- ground with 220# or 320#. It is important
loys is very low and therefore magnesium is that the force for grinding is also very low
added so that they can be age hardened. to avoid deep deformation and reduce fric-
tion between grinding foil/paper and sample
Cast alloys are produced by sand- chill- or surface; this can be relatively high for pure
die casting. Alloys with specific properties aluminium.
are used in various product groups for the
fabrication of pistons, slide bearings, parts Fig. 9: Aluminium-silicon cast, after polishing with 3µm
Diamond polishing has to be carried out
diamond small scratches are still visible, 200x.
for mechanical engineering, cylinder heads, until all deep scratches from grinding have
brake shoes etc. been removed.
In case water soluble constituents have to be
Some of the more important cast alloys and their
properties are listed:
identified, polishing with water free diamond
suspension and lubricant is recommended.
AlSi10Mg Age hardening, vibration and corrosion
resistant If diamond particles have been pressed into
AlSi5Cu1 Age hardening, good castebility, for the surface during polishing the following
welding, for thin section casting final polish with silicon dioxide suspension
AlMg3 Resistant against sea water can be relatively long (See Fig.1). Very often
AlSi25+ Cu Ni Age hardening, special alloy, for pistons, one can see already with the naked eye
wear resistant due to high Si content bright and dull areas on the samples sur-
AlMgSiPb Suitable for machining face. This is an indication that the final polish
AlSi9Cu3 Well castable universal alloy, most
Fig.10: Structure as in Fig. 9, but fine polished with
is not yet sufficient. It needs to be pointed
important alloy for pressure die casting
OP-U suspension. The matrix is well polished and the out that the embedded particles can lead to
eutectic has more contrast, 200x. erroneous interpretations of the structure.

Fig. 7: Aluminium-silicon cast, unrefined, 500x. Fig. 8: Aluminium-silicon cast, refined, 500x. Section of a mechanical engineering part
with aluminium cast components.
 quality control as it delivers fast and repro-
ducible results. For routine grain size deter-
mination at 100x, pre-grinding with 1000#

Pure Aluminium
Grinding
Step PG FG 1 FG 2 FG 3
Surface Foil/Paper* Foil/Paper* Foil/Paper* Foil/Paper*
Abra- Type SiC SiC SiC SiC
sive Size Fig.12: Plated sheet, anodised, grain areas are clearly
#320/500 #800 #1200 #4000 visible and suited for automatic image analysis, polari-
Fig.11: Aluminium-silicon cast polished too long Suspension Water Water Water Water sed light with λ¼-plate, 100x.
/ Lubricant
with OP-S suspension, silicon precipitates stand
in relief, 100x. Rpm 300 300 300 300
Force (N)/ 25 25 25 25
specimen
After 1 minute polishing with OP-U suspen-
Time (min) Until plane 0.5 0.5 0.5
sion the result is checked in the microscope.
If necessary the polish should be continued
for another minute and the result checked Polishing
again. It is recommended to continue this Step DP OP
* To avoid
polish /check sequence until the required Surface MD-Mol** MD-Chem coarse scrat-
quality of the result has been achieved. Type Diamond Collodial Silica ches, the
Abra-
sive
SiC-Foil/
Size 3 µm 0.04 µm Paper can be
(Approx. 20-30 sec before the end of polishing, water is rubbed with
Suspension DiaPro OP-U or OP-S
poured onto the polishing cloth to rinse the sample as / Lubricant Mol R3 wax before
well as the cloth. Then the sample is washed again with grinding. Fig.13: Pressed part, macro etching, primary and
Rpm 150 150
clean water from the tap and then dried. Note: Polishing **Alternatively heterogeneous precipitates are revealed that have a
Force (N)/ 25 15 MD-Dac negative effect on the surface of the final product.
too long with silicon dioxide suspension OP-S NonDry specimen
can cause a pronounced relief, see Fig.11). Time (min) 4 2-5
Electrolyte: A2
The following data are for the automatic Mask: 2 cm2
preparation of mounted specimens, 30 mm. Voltage: 39 V
Pure Aluminium, alternative method Flow rate: 10
Grinding Time: 20 sec.
Aluminium - Silicon Cast Step PG FG
Surface Foil/Paper* MD-Pan
Grinding After the polish, anodising with Barker’s
Type SiC Diamond
Step PG FG Abrasive reagent gives a colour contrast that is par-
Size #320 15 µm
ticularly suited for grain size evaluation. To
Suspension / Lubricant Water DiaPro Pan 15
Surface MD-Molto MD-Largo obtain the colour effect, polarised light with
Rpm 300 150
a λ¼ sensitive tint plate is used (Fig.12).
Abra- Type Diamond Diamond Force (N) / specimen 25 25
sive Size #220 9 μm Time (min) Until plane 5 Electrolyte: 200 ml water
Suspension / Water DiaPro Allegro/ 10 ml fluoroboric acid (35%)
Lubricant Largo 9 (Barker’s)
Rpm 300 150
Polishing
Mask: 2 cm2
Step DP OP
Voltage: 24 V
Force (N)/ 25 30 Surface MD-Dac 3 MD-Chem
specimen Flow rate: 8
or MD/Dur 3
Time (min) Until plane 4 Time: 1-2 min.
Type Diamond Collodial Silica
Abrasive
Size 3 µm 0.04 µm
Polishing DiaPro Etching and structure
Suspension / Lubricant OP-U or OP-S
Step DP OP
Dac 3/Dur 3 Macro etchants are used for grain size evalu-
Rpm 150 150 ation; also to show flow lines from extrusion
Surface MD-Mol* MD-Chem Force (N) / specimen 25 15 (Fig.13) and for revealing weld seams.
Time (min) 4 2-5
Before etching, the sample has to be ground
Abra- Type Diamond Collodial Silica to 1200# or 2400#.
sive Size 3 μm 0.04 μm *To avoid coarse scratches, the SiC-Foil/Paper can be
Suspension / DiaPro Mol R3 OP-U NonDry rubbed with wax before grinding. The many alloying possibilities of aluminium
Lubricant
result in a large variety of different phases
Rpm 150 150
that cannot always be clearly identified in
Force (N)/ 25 15 SiC-Foil/Paper is sufficient. Rolled or drawn some of the multi component alloys. Some
specimen surfaces do not need any grinding or polish- of the well known phases have the following
Time (min) 3 1 ing. For pure aluminium and precise exami- characteristic colours (see also Fig.6):
nations of grain shapes the samples have
*Alternatively MD-Dac. Si Grey
to be fine ground to 2000# and sometimes
Electrolytic Polishing is especially suited for even to 4000# before electrolytic polishing. Mg2Si Tarnished dark blue during polishing
(in cast: Chinese script)
pure aluminium and wrought alloys. It leaves Due to the many different phases in cast
Al2Cu Pinkish-brown, copper coloured
a scratch free surface and is often used in alloys, they are not suited for electrolytic
polishing. Al6Mn Light grey
 Struers ApS
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Fig.15: Experimental aluminium alloy with 6% Si and Fig.16: Same as Fig.15 but etched for 30 sec with 1g [email protected]
10% copper, unetched. molybdic acid in 200 ml water + 6 g ammonium www.struers.com
chloride. The silicon is dark blue and is distinguishable
Depending on the alloying content, these from the greyish CuAl2.
eutectic phases can sometimes be recog- AUSTRALIA & NEW ZEALAND
Struers Australia
NETHERLANDS
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nised by the typical shape of their eutectic. determination, evaluation of phases, impuri- 27 Mayneview Street Zomerdijk 34 A
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The relevant literature lists etchants which ties and mechanical defects. Pure aluminium Australia Telefoon +31 (10) 599 7209
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can be used to identify these phases (Fig.15 is very susceptible to deformation and there- Fax +61 7 3369 8200 [email protected]
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Wrought alloys with a heavily deformed with silicon dioxide suspension is necessary 370, rue du Marché Rollay 1407 Vinterbro
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Acknowledgements [email protected]
standard safety precautions have to be SWITZERLAND
We wish to thank AMAG rolling GmbH, Ranshofen, CZECH REPUBLIC & SLOVAKIA Struers GmbH
observed. Struers GmbH Organizační složka Zweigniederlassung Schweiz
Austria, for supplying sample material and for the vědeckotechnický park Weissenbrunnenstraße 41
permission to reproduce the photo with the lamps on Přílepská 1920, CH-8903 Birmensdorf
Macro etching page 3. Our special thanks go to Ms. Petra Mersch and CZ-252 63 Roztoky u Prahy Telefon +41 44 777 63 07
Phone +420 233 312 625 Fax +41 44 777 63 09
For pure aluminium 90 ml water Dr. Reinhardt Rachlitz for their support. Fax +420 233 312 640 [email protected]
15 ml hydrochloric acid [email protected]
We wish to thank Austria Alu-Guss-Gesellschaft G.m.b.H., [email protected] SINGAPORE
10 ml hydrofluoric acid Ranshofen, Austria, for the permission to reproduce the Struers Singapore
photo of the aluminium wheel rim on page 1. GERMANY 627A Aljunied Road,
Deep etching to reveal the primary dendritic structure Struers GmbH #07-08 BizTech Centre
100 ml water We wish to thank Thomas Zwieg, Danish Institute of Carl-Friedrich-Benz-Straße 5 Singapore 389842
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10-25 g sodium hydroxide Technology, Aarhus, Denmark, for the permission to Telefon +49 (0) 2154 486-0 Fax +65 6299 2661
reproduce Fig.17. Fax +49 (0) 2154 486-222 [email protected]
[email protected]
Micro etching SPAIN
Bibliography FRANCE Struers España
Flick’s reagent: Struers S.A.S. Camino Cerro de los Gamos 1
Structure 38, Thomas, Zwieg, Danish Institute of 370, rue du Marché Rollay Building 1 - Pozuelo de Alarcón
Grain boundary etching for most types of aluminium
Technology, Aarhus, Denmark, A universal method F-94507 Champigny CP 28224 Madrid
and alloys sur Marne Cedex Teléfono +34 917 901 204
for the mechanical preparation of aluminium alloy
90-100 ml water Téléphone +33 1 5509 1430 Fax +34 917 901 112
0.1-10 ml hydrofluoric acid specimens with high edge retention and their Télécopie +33 1 5509 1449 [email protected]
subsequent colour etching. [email protected]
FINLAND
Dix and Keller reagent: Structure 8, Etching of aluminium alloys, Dr. Philippe HUNGARY Struers ApS, Suomi
Grain area etching for Al-alloys with copper, also suitable Lienard, Pof. Clement Pacque, Faculte Polytechnique de Struers GmbH Hietalahdenranta 13
Magyarországi Fióktelepe 00180 Helsinki
for pure aluminium. Mons, Belgien. 2040 Budaörs Puhelin +358 (0)207 919 430
190 ml water Szabadság utca 117 Faksi +358 (0)207 919 431
ASM Handbook, Vol. 9, Metallography and Phone +36 2380 6090 [email protected]
5 ml nitric acid
10 ml hydrochloric acid Microstructures, ASM, 2004. Fax +36 2380 6091
Email: [email protected] SWEDEN
2 ml hydrofluoric acid Metals Handbook, Desk Edition, ASM, 1997. Struers Sverige
IRELAND Box 20038
Informationsmaterial des Gesamtverbands Deutscher Struers Ltd. 161 02 Bromma
Colour etchants: Molybdic acid solution according Metallgießereien e.V., Düsseldorf. Unit 11 Evolution@ AMP Telefon +46 (0)8 447 53 90
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