Metallographic Techniques For Aluminum and Its Alloys

ASM Handbook, Volume 9: Metallography and Microstructures Copyright © 2004 ASM International®
G.F. Vander Voort, editor, p711–751 All rights reserved.

DOI: 10.31399/asm.hb.v09.a0003769 Color images cited in this article appear at end of article. www.asminternational.org
Metallographic Techniques for

Aluminum and Its Alloys
Małgorzata Warmuzek, Foundry Research Institute, Kraków, Poland
ALUMINUM ALLOYS encompass a wide ● The embedding of abrasive particles in the phous compounds, and arrays of different con-
range of chemical compositions and product metal during polishing is more likely. tinuous solid solutions. The following section
forms that can be manufactured by all available ● Relief between the matrix and second-phase briefly describes the function of major alloying
metalworking techniques and standard casting particles, which are considerably harder than elements, phase formation, and the morpholo-
processes. Manufactured forms of aluminum and the matrix, develops more readily during pol- gies of constituents formed by liquid-solid or
aluminum alloys include standard mill products ishing. solid-state transformations. Structure and prop-
(e.g., sheet, plate, foil, rod, bar, wire, tube, pipe, erties of aluminum alloys are also described in
and structural forms) and engineered forms for Harder alloys, although easier to prepare, more detail in Ref 1 to 3.
specific applications produced by extrusion, present a greater variety of phases and complex-
forging, stamping, powder metallurgy, semisolid ities of structure. In all cases, the procedures for
processing, and machining. Aluminum products sample collection and preparation must consider Composition and Phases
also include metal-matrix composites with either specific mechanical and structural properties,
particulate or fiber reinforcement. This article fo- such as the high difference of hardness between Aluminum alloys encompass more than three
cuses primarily on the metallography and micro- matrix and other phase constituents and the rela- hundred commonly recognized alloy composi-
structures of wrought and cast forms. Powder tively low temperature of the precipitation pro- tions and many additional variations developed
metallurgy, semisolid processing, and composite cesses in the solid state. in supplier/consumer relationships. All commer-
forms are discussed in other articles of this Vol- Information taken from the structural images cial aluminum alloys contain some iron and sil-
ume. allows the formation of a qualitative or quanti- icon as well as two or more elements intention-
Metallographic preparation of aluminum al- tative description of bulk (average) structure or ally added to enhance properties. The main
loys may vary considerably due to the wide specific local features in terms of spatial distri- groups of commercial aluminum alloys of dif-
range of chemical compositions and resulting bution, dispersion, morphology, and volume ferent chemical composition are presented in Ta-
hardness. Softer alloys generally are more diffi- fraction of all the phase constituents. The inter- ble 1. The principal types of aluminum alloys
cult to prepare by mechanical polishing, be- pretation of aluminum alloy microstructures re- achieve strengthening by the alloying effects of
cause: quires an understanding of the various morpho- copper, magnesium, manganese, silicon, and
● Deformation caused by cutting and grinding logical forms and the simultaneous presence of zinc (Fig. 1) in conjunction with strain harden-
extends to a greater depth. the stable and metastable constituents, isomor- ing, heat treatment, or both.
Table 1 Alloy composition range for major groupings of commercial aluminum alloys
Nominal chemical composition(a), wt%
Alloy group Mg Si Ti Cr Mn Fe Ni Cu Zn Zr Other
Wrought alloys
1xxx (Al 99.00%) 0.006–0.25 0.006–0.7 0.002–0.06 0.01–0.03 0.002–0.05 0.006–0.6 ... 0.006–0.35 0.006–0.05 ... ...
2xxx (Cu) 0.02–0.8 0.10–1.3 0.02–0.3 0.05–0.2 0.05–1.3 0.12–1.3 0.05–2.3 0.8–6.8 0.10–0.80 0.05–0.5 ...
3xxx (Mn) 0.05–1.3 0.3–1.8 0.05–0.10 0.05–0.40 0.05–1.8 0.1–1.0 0.05 0.05–0.50 0.05–1.0 0.1–0.5 ...
4xxx (Si) 0.05–2.0 0.8–13.5 0.04–0.30 0.05–0.25 0.03–1.5 0.20–1.0 0.15–1.3 0.05–1.5 0.05–0.25 ... ...
5xxx (Mg) 0.2–5.6 0.08–0.7 0.05–0.20 0.05–0.35 0.03–1.4 0.10–0.7 0.03–0.05 0.03–0.35 0.05–2.8 ... ...
6xxx (Mg Ⳮ Si) 0.05–1.5 0.20–1.8 0.08–0.20 0.03–0.035 0.03–1.0 0.08–1.0 0.2 0.10–1.2 0.05–2.4 0.05–0.20 ...
7xxx (Zn) 0.10–3.7 0.10–0.50 0.03–0.15 0.04–0.35 0.02–1.5 0.10–0.70 0.10 0.05–2.6 0.8–8.7 0.05–0.18 ...
8xxx (other element) 0.02–1.4 0.10–1.0 0.08–0.2 0.01–0.2 0.02–1.0 0.10–2.0 0.2–1.3 0.03–2.2 0.03–1.8 0.04–0.16 Li, B, Sn, Ga
Cast alloys
1xx.x (Al 99.00%) ... 0.10–0.15 0.15–0.35 ... ... 0.25–0.8 ... 0.05–0.10 0.05 ... ...
2xx.x (Cu) 0.03–2.3 0.05–3.5 0.06–0.35 0.15–0.40 0.05–0.7 0.04–1.5 0.03–2.3 3.5–10.7 0.05–2.5 ... ...
3xx.x (Si Ⳮ Cu/Mg) 0.03–1.5 4.5–23.0 0.04–0.25 0.05–0.35 0.03–0.8 0.06–1.5 0.10–3.0 0.03–5.0 0.03–4.5 ... ...
4xx.x (Si) 0.05–0.10 3.3–13 0.20–0.25 0.25 0.05–0.5 0.12–1.3 0.05–0.5 0.05–1.0 0.05–0.5 ... ...
5xx.x (Mg) 1.4–10.6 0.10–2.2 0.10–0.25 0.25 0.05–0.6 0.10–1.3 0.05–0.4 0.05–0.30 0.05–0.20 ... ...
7xx.x (Zn) 0.2–2.4 0.10–0.30 0.10–0.25 0.06–0.6 0.05–0.6 0.10–1.4 0.15 0.1–1.0 2.0–7.8 ... ...
8xx.x (Sn) 0.1–0.9 0.4–6.5 0.2 ... 0.1–0.5 0.5–0.7 0.3–1.5 0.7–4.0 Sn, 5.5–7.0 ... ...
(a) bal aluminum. Source: Ref 1, 2
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712 / Metallography and Microstructures of Nonferrous Alloys
Phase Formation and Morphology ever, silicon or tin may form intermetallic-com- phase is cooled below the solvus line, dispersed
pound phases. Al2Cu particles precipitate, depleting copper
Some common phase constituents present in Most of the other alloying elements form such from the ␣ solid solution. When cooled to room
the numerous commercial aluminum alloys are intermetallic compounds with aluminum in bi- temperature under near-equilibrium (slow) con-
shown in Tables 2 and 3 (Ref 2–6). In general, nary alloys and more complex phases in ternary ditions, the ␣ solid solution contains little cop-
the phases may develop various morphologies or higher-order alloys. In the aluminum-copper per, so strength is low. To increase strength, the
with resulting microstructures that can range system, for example, when the ␣ solid-solution material must be solution heat treated, quenched,
from a simple monophase (solid-solution) struc-
ture to various polyphase morphologies (Fig. 2).
The occurrence of these various morphologies,
which can have a strong influence on properties,
depends on alloy concentration and solubility
and how the phases form during solidification
and/or solid-state heat treatment.
The aluminum-copper phase diagram (Fig. 3),
which includes the commercially important class
of 2xxx aluminum alloys, can illustrate the basic
alloying regions of phase formation. The three
important regions of phase formation are:
● The solid-solution (␣) region (below 0.1 wt%
Cu), where the alloying atoms remain dis-
solved by substituting aluminum atoms in the
aluminum/face-centered cubic (fcc) lattice. In
this alloying region, the terminal (room-tem-
perature) solid-state condition is essentially a
monophase structure (Fig. 4).
● The solid-state region below the solvus line,
where dispersed particles of the h (Al2Cu) in-
termetallic precipitate in a supersaturated alu-
minum-copper solid
● The region to the right of the maximum solid-
Fig. 1 The principal alloying elements of aluminum alloys. Source: Ref 2
solubility point (5.65 wt% Cu), where the
h(Al2Cu) phase precipitates during solidifi-
cation and thus forms a network of second-
phase particles around the previously solidi- Table 2 Phase constituents present in commercial aluminum alloys
fied ␣ grains in the L Ⳮ ␣ region Phase constituents(a)
Alloy Rough state Treated state
The latter two reactions have an important influ-
ence on the morphology of the second-phase par- Wrought alloys
ticles. When phase precipitation occurs during a 1xxx (Al 99.00%), Al-Fe-Si, Al-Cu Al3Fe, ␣-Al(FeSi) Al6Mn, ␣-Al(FeSi)
liquid-solid transformation (such as for eutectic 2xxx (Cu), Al-Si-Cu-Mn-Mg, Al-Si- Al2Cu, Al2CuMg, Al20Cu2Mn3, ␣- Al2Cu, Al2CuMg, Al20Cu2Mn3, ␣-
Cu-Mn, Al-Cu-Mg, Al-Cu-Mg-Ni, Al(FeMnSi), Al3FeMn, Al6MnFe, Al(FeMnSi), Al7Cu2Fe, Al12Mn3Si
reactions described subsequently), the precipi- Al-Cu-Mn-Ti-V-Zr, Al-Cu-Mg-Ni- Al7Cu2Fe, Mg2Si, Al5Cu2Mg8Si6
tates form a networklike morphology by solidi- Fe-Ti
fying around the ␣ grains. In contrast, solid-state 3xxx (Mn), Al-Cu-Mn, Al-Fe-Si-Mg- ␣-Al(FeMnSi), Al6MnFe ␣-Al(FeMnSi), Al6MnFe
processes tend to produce a more dispersed sec- Mn, Al-Si-Mn- Fe
4xxx (Si) b-AlFeSi ...
ond phase, such as those shown in Fig. 5 at vari- 5xxx (Mg), Al-Mn-Mg-Cr, Al-Mn- Mg2Si, Al18Mg3Cr2, Al6Mn Mg2Si, Al3Ni
ous levels of magnification. Mg-Cr, Al-Mn-Mg, Al-Mg
Solid-state precipitation occurs when element 6xxx (Mg, Si), Al-Si-Cu-Mg-Cr, Al- b-AlFeSi, Mg2Si, ␣-Al(FeSi) Mg2Si
concentrations exceed their solid solubility dur- Si-Mg, Al-Si-Mg-Cr, Al-Si-Mn-Mg
7xxx (Zn), Al-Mn-Mg-Zn-Zr, Al-Mn- ␣-Al(FeCrSi), Al2CuMgZn, Al7Cu2Fe Al2CuMg, Mg2Si, Al7Cu2Fe, ␣-
ing cooling. The solubility limits of alloying ele- Mg-Cr-Zn, Al-Zn, Al-Cu-Mg-Cr- Al(FeCrSi), Al18Mg3Cr2
ments in solid aluminum are very low (Table 5), Zn, Al-Cu-Mn-Mg-Cr-Zn, Al-Cu-
and no element is known to have complete mis- Mg-Cr-Zn
cibility with aluminum in the solid state. Com- 8xxx (other element), Al-Li-Mg-Cu ... ...
mercially pure aluminum is a pure solid-solution Cast alloys
(monophase) material (Fig. 4). Among the com- 1xx.x (Al 99.00%), 7xxx(Zn) Si, b-AlFeSi, ␣-Al(FeSi) ...
mercial alloys, only the bright-finishing alloys 2xx.x (Cu), Al-Cu-Mg, Al-Cu-Mn, Si, Al2Cu, Al2CuMg, Al7Cu2Fe, Al2Cu, Al2CuMg, Al20Cu2Mn3,
such as 5657 and 5252, which contain 0.8 and Al-Cu-Si-Mg, Al-Cu-Mn-Mg-Ni, Al5Cu2Mg8Si6, b-AlFeSi Al7Cu2Fe, AlCuFeNi, Al6Cu3Ni,
Al-Cu-Mg-Ni, Al-Cu-Si ␣-Al(FeMnSi), AlCuFeNi, Al6Cu3Ni Al3Ni
2.5% Mg (nominal), respectively, with very low 3xx.x (Si Ⳮ Cu/Mg), Al-Cu-Si, Al- Si, Al2Cu, Al2CuMg, Al7Cu2Fe, Si, Al2Cu, Al2CuMg, Al7Cu2Fe,
limits on all impurities, may be regarded as Si-Cu-Mg-Ni, Al-Si-Cu-Mg, Al-Si- Al5Cu2Mg8Si6, b-AlFeSi AlCuFeNi, Al6Cu3Ni, Al20Cu2Mn3,
nearly pure solid solutions. When the content of Mg, Al-Si-Mg-Fe, Al-Si-Mg-Ti, ␣-Al(FeMnSi), AlCuFeNi, Al6Cu3Ni, Al3Ni, Al8Mg3FeSi2,
an alloying element exceeds the solid-solubility Al-Si-Mn-Mg-Cu Mg2Si, Al3Ni, Al9NiFe, Al5Cu2Mg8Si6, b-AlFeSi,
Al8Mg3FeSi2 ␣-Al(FeMnSi)
limit, the alloying element produces second- 4xx.x (Si), Al-Si, Al-Si-Cu, Al-Si-Fe Si, Al2Cu, b-AlFeSi, ␣-Al(FeMnSi) Si, Al2Cu, b-AlFeSi, ␣-Al(FeMnSi)
phase microstructural constituents. Second- 5xx.x (Mg), Al-Mg Mg2Si, Al6(FeMn), Al3Mg2, Mg2Si, Al6(FeMn), Al3Mg2,
phase constituents may consist of pure element Al18Mg3Cr2 Al18Mg3Cr2
precipitates or mainly intermetallic phases. In 7xx.x (Zn) Al18Mg3Cr2, Al3Fe, Al7FeCr, MgZn2 ...
8xx.x (Sn) Si, Sn, Cu6Sn5, Al3Ni Si, Sn, Cu6Sn5, Al3Ni, Al6Cu3Ni
the first group are silicon, tin, and beryllium. If
the alloy is a ternary or higher-order alloy, how- (a) ␣-Al(other) ⳱ solid solution. Source: Ref 2–6

Metallographic Techniques for Aluminum and Its Alloys / 713
Table 3 Characteristics of phase constituents in aluminum-rich aluminum alloys

Crystal lattice
Chemical composition(a)
Cell parameters,
Phase System, space group Angstroms wt% at.% Morphology of precipitates
Si Cubic, A4 a ⳱ 5.43054 100 100 Polyhedra, branched platelets, or rods
Sn Tetragonal, Fd3m a ⳱ 5.8318 100 100 Irregular, compact particles
c ⳱ 3.1819
Al Cubic, fcc a ⳱ 4.0333 100 100 Matrix of alloy grains, dendrites
AlAg2 Hexagonal, P6/mmc a ⳱ 2.885 88.9% Ag 66.6% Ag Dispersed particles
c ⳱ 4.582
Al9Co2 Monoclinic, P21/c a ⳱ 6.213 32.7% Co 18.2% Co Irregular plates
b ⳱ 6.29
c ⳱ 8.556
b ⳱ 94 76⬘
Al2Cu Tetragonal, I4/mcm a ⳱ 6.066 52.5–53.9% Cu 33.3% Cu Round or irregular particles,
c ⳱ 4.874 dispersed particles
Al7(CrFe) Orthorhombic a ⳱ 24.8 21.6% Cr 12.5% (Fe,Cr) Irregular, faceted polyhedra, needles
b ⳱ 24.7
c ⳱ 30.2
Al12(CrMn) Cubic, bcc, Im3 a ⳱ 7.507 2–4% Cr, 10–12% Mn 7.7% (CrMn) Irregular, compact particles
Al3Fe Monoclinic, C2/m a ⳱ 15.520 40.8% Fe 25% Fe Needles or rosettes
b ⳱ 8.099
c ⳱ 12.051
b ⳱ 107
Al6Fe Orthorhombic, Ccmm a ⳱ 6.464 25.65% Fe 14.3% Fe Platelets or rods
b ⳱ 7.440
c ⳱ 8.779
␣(FeCu) Ccm21 7–8% Cu, 22–25% Fe Platelets
Al3Mg2 Cubic, fcc, Fd3m a ⳱ 28.16 34.8–37.1% Mg 40% Mg Compact, rounded particles, outlining
grains
AlLi Cubic, bcc, Fd3m a ⳱ 6.38 20.5% Li 50% Li Dispersed particles at grain
boundaries
Al6Mn, Al6(MnFe) Orthorhombic, Cmcm a ⳱ 6.498 25.34% Mn 14.3% Mn Parallelograms, more or less
b ⳱ 7.552 elongated
c ⳱ 8.870
Al3Ni Orthorhombic a ⳱ 6.611 42% Ni 25% Ni Branched polyhedra
b ⳱ 7.366
c ⳱ 4.812
Al3Ti Tetragonal, I4/mmm a ⳱ 3.848 36.5–37.5% Ti 25% Ti Platelets
c ⳱ 8.596
AlSb Cubic, F43m a ⳱ 6.096 81.9% Sb 50% Sb Compact particles
Al6V Hexagonal, P63/mmc a ⳱ 7.718 23.8% V 14.3% V Dispersed particles
c ⳱ 17.15
Al11V Cubic, Im3 a ⳱ 14.586 15.1–15.9% V 8.3% V Dispersed particles
Al3Zr Tetragonal, I4/mmm a ⳱ 4.018 53.0% Zr 25% Zr, bal Al Compact particles
c ⳱ 17.320
Mg2Si Cubic, fcc, Fm3m a ⳱ 6.351 63.2% Mg, 36.8% Si 66.6% Mg, 33.3% Si Fine Chinese script,
Hexagonal, b⬘ a ⳱ 7.05 dispersed particles
c ⳱ 4.05
MgZn2, AlCuMg Hexagonal, P63/mmc a ⳱ 5.18 15.68% Mg, 84.32% Zn 33.3% Mg, 66.6% Zn Irregular round particles,
c ⳱ 8.517 dispersed particles
a ⳱ 5.07 55.7% Cu, 20.8% Mg 33.3% Mg, 33.3% Cu
c ⳱ 8.29
Mg2Zn11- Cubic, Pm3 a ⳱ 8.552 56.4% Cu, 9.2% Mg 15.4% Mg, 74.6% Zn Irregular round particles,
Al5Mg2Cu6 c ⳱ 8.311 46.2% Cu, 6.67% Mg dispersed particles
TiB2 Hexagonal, P6/mmm a ⳱ 3.028 68.9% Ti, 31.1% B 33.3% Ti, 66.7% B Irregular particles
c ⳱ 3.228
Al18Cr2Mg3 Cubic, Fd3m a ⳱ 14.53–14.65 15.7(11–13)% Cr, 11.1(8–12)% Mg 8.7% Cr, 13.0% Mg Chinese script
Al7Cu2Fe Tetragonal, P4/mnc a ⳱ 6.33 36.9% Cu, 16.2% Fe 10% Fe, 20% Cu Thin needles
c ⳱ 14.81
Al2CuLi Hexagonal a ⳱ 4.96 52.8% Cu, 5.4% Li 25% Cu, 25% Li Dispersed particles
c ⳱ 9.35
Al6CuMg4, Al2Mg3Zn3 Cubic, bcc, Im3 a ⳱ 14.15 22–27% Cu, 27.5–30% Mg 9.1% Cu, 36.4% Mg Irregular, round particles
Al20Cu2Mn3 Orthorhombic, Cmcm a ⳱ 24.11 12.8–19% Cu, 19.8–24% Mn ... Irregular, compact particles
b ⳱ 12.51
c ⳱ 7.71
Al7Cu4Ni Varied with composition ... 47–50.6% Cu, 12.1–12.5% Ni ... Irregular, elongated particles,
skeleton-like
Al9FeNi Monoclinic, P21/c a ⳱ 6.2 4.5–14% Fe, 18–28% Ni ... Branched, elongated polyhedra
b ⳱ 6.3
c ⳱ 8.6
␣ ⳱ 95
b-AlFeSi Monoclinic a ⳱ 6.12 25–30% Fe, 12–15% Si 14.3% Fe, 14.3% Si Needles
b ⳱ 6.12
c ⳱ 41.48
␣ ⳱ 91
␣-AlFeSi Hexagonal, P6/mmc a ⳱ 12.3 30–33% Fe, 6–12% Si 9.1% Si, 18.2% Fe Chinese script
c ⳱ 26.3
(continued)
Note: fcc, face-centered cubic; bcc, body-centered cubic. (a) Bal aluminum. Source: Ref 3–5

Table 3 (continued)
Crystal lattice
Chemical composition(a)
Cell parameters,
Phase System, space group Angstroms wt% at.% Morphology of precipitates
c-AlFeSi Monoclinic, Cfc a ⳱ 17.8 33.9% Fe, 16.9% Si, bal Al 20% Fe, 20% Si Platelets or needles
b ⳱ 10.25
c ⳱ 8.90
b ⳱ 132
d-AlFeSi Tetragonal a ⳱ 6.16 25.4% Fe, 25.5% Si 14.3% Fe, 28.6% Si Platelets
c ⳱ 9.49
␣-AlMnSi Cubic, Pm3 a ⳱ 12.652 26.3% Mn, 8.9% Si 15% Mn, 10% Si Chinese script, polyhedra
␣-AlFeMnSi Cubic, Im3 a ⳱ 12.50 33% (FeMnCr), 5.97% Si 19.2% (FeMnCr), 7.7% Si Polyhedra, Chinese script
Al4CuMg5Si4 bcC a ⳱ 12.63
Al5Cu2Mg8Si6 Hexagonal a ⳱ 10.32 10.16% Cu, 31.1% Mg, 17.7% Si 28.5% Si, 38.1% Mg, 9.5% Cu Round or irregular particles
c ⳱ 4.05
Al8Mg3FeSi2 Hexagonal, P62m a ⳱ 6.63 18.2% Mg, 13.9% Fe, 14.1% Si 14.3% Si, 21.4% Mg, 7.1% Fe Chinese script
c ⳱ 7.94
Note: fcc, face-centered cubic; bcc, body-centered cubic. (a) Bal aluminum. Source: Ref 3–5
and aged to develop metastable precipitates. most of the copper remains in liquid form. As In the aluminum-copper system, a network of
During fast cooling, the ␣ solid solution is su- the temperature approaches the solidus, the ␣ the Al2Cu intermetallic can be detrimental, de-
persaturated, and then, as a result of its tendency solid phase becomes more enriched with copper. pending on the extent and coarseness of the
to achieve thermodynamic equilibrium, the When the temperature falls below the solidus Al2Cu particles. In addition, it is also important
Al2Cu intermetallic precipitates as dispersed par- temperature in alloys containing less than the to realize that the eutectic reaction can occur in
ticles. maximum solubility (5.65 wt% Cu), solidifica- alloys containing less than the maximum solid
Among the intermetallic phases, several tion is complete to the solid-solution phase con- solubility under commercial casting conditions,
groups can be mentioned: dition (␣). In alloys containing more than 5.65 even though the equilibrium phase diagram does
wt% (2.5 at.%) Cu, some liquid remains when not predict that. Consequently, Al2Cu particles
● Electron compounds (Hume Rothery phases)
the eutectic temperature (548 C, or 1018 F) is form during solidification of most aluminum al-
● Laves phases
reached. In this case, two terminal solid-solution loy ingots and shaped castings. Therefore, they
● Intermediate solid-solution phases
phases (␣ and h) separate out simultaneously are preheated or homogenized to dissolve the in-
The morphology and thermophysical properties from the molten liquid. On cooling below the termetallic particles.
of the intermetallic phase particles can influence eutectic temperature, a network of eutectic forms Various types of as-cast morphologies are ob-
the properties of the alloy at different steps of in the residual liquid surrounding the dendrites tained, depending on whether the alloy content
production or processing. Essentially, the inter- or grains of primary ␣. is above, below, or near the eutectic composi-
mediate solid-solution phases occur when the
crystal lattice of the base metal cannot accom-
modate any more atoms of the alloying element.
When this occurs, a new phase forms with a dif-
ferent crystal structure that can more easily ac-
commodate the undissolved alloying atoms.
Liquid-Solid Transformations. The eutectic
and peritectic reactions are the two major forms
of liquid-solid transformation in aluminum al-
loys, and examples of each are briefly described
in terms of equilibrium phase diagrams and
phase morphology. Although few products are
sold and used in their equilibrium condition,
equilibrium phase diagrams are essential in un-
derstanding the effects of composition and both
solidification and solid-state thermal processing
on microstructure. For aluminum alloys, phase
diagrams are used to determine solidification and
melting temperatures, the solidification path, and
the equilibrium phases that form and their dis-
solution temperatures. In addition to determining
appropriate temperatures for casting and thermal
treatments, phase diagrams are used to determine
the maximum levels for ancillary element addi-
tions of certain elements to prevent the crystal-
lization of coarse primary particles.
Eutectic Reaction. The aluminum-copper di-
agram (Fig. 3) and the aluminum-silicon dia-
gram (Fig. 6) are two examples of simple eutec-
tic systems. Using the aluminum-copper system
as an example, the basic process of solidification
and morphology formation is as follows. When Fig. 2 Typical microstructure morphologies. (a) Solid-solution monophase typical of commercially pure (1xxx and
1xx.x) aluminum alloys. (b) Dispersed second phase typical of deformed and heat treated wrought aluminum
the temperature goes below the liquidus line, the alloys. (c) Continuous network of second phases typical of alloys in an as-cast condition. (d) Discontinuous network of
solid-solution phase (␣) solidifies first, while second-phase particles in heat treated cast or wrought alloys. (e) Duplex microstructure

tion. This is shown for the aluminum-silicon sys- conditions, however, the primary particles of of these soluble constituents dissolve either dur-
tem (Fig. 6). Hypoeutectic aluminum-silicon al- Al7Cr would not have the opportunity to trans- ing ingot preheating prior to deformation pro-
loys (i.e., those with alloying contents below the form to ␣ solid solution, so they would remain. cessing or during the solution heat treatment of
eutectic composition of 12.6 wt% Si) have a net- Consequently, maximum chromium limits are cast shapes or wrought products. Constituent
work structure of a second phase (gray) that sur- established so that all of the chromium remains size decreases with increasing solidification rate.
rounds grains of solid-solution aluminum (light). in supersaturated solid solution in the ingot. It In hypoeutectic 3xx.0 and 4xx.0 castings, modi-
Similar as-cast structures are shown in Fig. 7 for precipitates as chromium-bearing dispersoids fication by elements such as strontium signifi-
two other hypoeutectic alloys. In the case of eu- during ingot preheat. Micrographs of two other cantly refine the flake structure of the silicon par-
tectic and hypereutectic compositions, the as- peritectic structures in Al-Fe(Mn)-Si and Al-Fe- ticles to a finer fibrous morphology. Constituent
cast structure may have mixed morphologies of Cu-Ni systems are shown in Fig. 14. particles are generally not beneficial.
both networklike and dispersed second phases. Second-phase particles are divided into four Dispersoids form by solid-state precipitation,
In these cases, a dispersed second phase may oc- classes, based on their mode of formation and either during ingot preheating or during the ther-
cur as a primary product during solidification their ability to be dissolved: primary particles, mal heat treatment of cast shapes of slow-diffus-
above the eutectic temperature. These types of constituents, dispersoids, and precipitates. ing supersaturated elements that are soluble in
mixed as-cast morphologies are shown in Fig. 8 Primary particles refer to the solid phase that molten aluminum but that have limited solubility
and 9 for some eutectic and hypereutectic alloys, separates first from the melt. For example, pri- in solid aluminum. Manganese, chromium, or
respectively. Phase morphologies also can be mary silicon particles form first in the L Ⳮ Si zirconium are typical dispersoid-forming ele-
modified either during the solidification process phase of hypereutectic aluminum-silicon alloys ments. Unlike the precipitates that confer pre-
or by solid-state processing (such as bulk work- (Fig. 6). The coarse, faceted primary silicon par- cipitation hardening, dispersoids are virtually
ing and/or heat treatment). For example, Fig. 10 ticles are refined to a fine, spherulitic structure impossible to dissolve completely, once precip-
is the as-cast structure of aluminum-silicon eu- using additives containing phosphorus. In cer- itated. In addition to providing dispersion
tectic with and without alloy modification during tain casting alloys and 8xxx wrought alloys, pri- strengthening, the size distribution of disper-
liquid processing. Modification of morphology mary iron-bearing constituents can form if the soids in wrought alloys is a key factor in con-
by heat treatment is shown in Fig. 11 and 12. alloying content is such that the alloy is hyper- trolling degree of recrystallization, recrystallized
Peritectic Reaction. The aluminum-chromium eutectic. In wrought alloys, macroscopically grain size, and crystallographic texture. Disper-
system (Fig. 13) is an example of a peritectic large, undesirable primary particles of Al7Cr, soids in non-heat-treatable alloys also stabilize
system. During equilibrium solidification of al- Al3Ti, or Al3Zr can form by a peritectic reaction the deformation substructure during elevated-
loys containing more than the peritectic com- if chemical composition is not closely con- temperature exposures, for example, during
position (0.41% Cr but less than the maximum trolled. paint baking.
solid solubility of 0.77%), an intermetallic com- Constituents. These particles may be either in- In contrast to the commercially significant dis-
pound, Al7Cr, forms when the liquidus tempera- termetallic compounds or metal crystals that persion strengthening provided by dispersoids in
ture is reached. When the temperature falls to the form during solidification of hypoeutectic alloys. 3xxx and 5xxx alloys, the level of dispersion
peritectic temperature, 661 C (1222 F), the re- They range in size from a few micrometers to strengthening afforded by dispersoids in
maining liquid along with the Al7Cr transforms tens of micrometers. Constituents can be classi- wrought heat treatable alloys is trivial. In 2x24
to ␣-aluminum. Under commercial solidification fied either as virtually insoluble or soluble. Most alloys, Al20Cu2Mn3 dispersoids nucleate dislo-
cations at the particle-matrix interface during the
quench. These dislocations serve as nucleation
sites for subsequent precipitation. The newer
7xxx alloys contain zirconium, which forms co-
herent Al3Zr dispersoids, while most of the older
7xxx alloys contain Al12Mg2Cr dispersoids,
which exhibit incoherent interfaces. The inco-
herent interfaces serve to nucleate MgZn2 pre-
cipitates during the quench, so alloys containing
these precipitates lose a great deal of their po-
tential to develop high strength after slow
quenching (quench sensitivity). Nucleation is
difficult on coherent interfaces, so the newer al-
Fig. 4 Monophase structure of etched commercially

Fig. 3 Aluminum corner of the aluminum-copper phase diagram. Eutectic composition (not shown) is at 33 wt% (17 pure aluminum (1xx.x) at 200⳯ magnification.
at.%) Cu. HF etchant (5m in Table 4)

loys are less quench sensitive. A number of cast- Table 4 Reagents for chemical microetching
ing alloys, and some wrought alloys, contain ele- No. Chemical composition Etching mode Purpose or application Ref
ments that can form either constituents or
1m 25 mL HNO3 (70%) 70 C (160 F), 40 s Phase identification, 7–10
dispersoids, depending on the solidification rate. 75 mL distilled H2O especially in Al-Cu alloys
Precipitates can form during any thermal 2m 20 mL H2SO4 (98%) 70 C (160 F), 30 s Phase identification, Al-Cu, 7–11
operation below the solvus. In properly solution- 80 mL distilled H2O 30 s–3 min Mn, Mg, Fe, Be, Ti alloys
heat-treated products, all precipitates dissolve 3m 1 g NaOH 50 C (120 F), 5–15 s Phase identification; 8–10
100 mL distilled H2O Clean in 5% HNO3, rinse in AlCuMgZn alloys need 2–
during the solution-heat-treatment operation. cold water, prepare fresh 3 min etching.
Depending on quench rate and alloy, precipitates before use
can form during the quench from the solution- 1 g NaOH Swab 5–10 s 7
heat-treatment temperature at grain and subgrain 100 mL distilled H2O
4m 10 g NaOH 70 C (160 F), 5 s Phase identification 8, 11
boundaries and at particle-matrix interfaces. 100 mL distilled H2O Prepare fresh before use
These coarse precipitates do not contribute to 5m 0.5 mL HF (40%) At ambient temp., 5–60 s to Phase identification; reveals 5, 8–13
age hardening and can serve to reduce properties 100 mL distilled H2O alternately polish and etch grain boundaries, slip lines
such as ductility, fracture toughness, and resis- (The HF concentration can be increased several times in pure Al
up to 10 mL).
tance to intergranular corrosion. After the Toxic!
quench, Guinier-Preston (GP) zones form at am- 6m 5 mL HF (40%) At ambient temperature, 5– Phase identification 8, 11
bient temperature (natural aging). These are ag- 15 mL HCl (38%) 60 s
glomerates of atoms of the major solute elements 25 HNO3 (70%)
955 mL distilled H2O
with a diffuse, coherent boundary between the 7m A) 2(4) mL HF (40%) At ambient temperature, 10– Al and Al alloys (Al-Si cast 9, 10
GP zone and the matrix. During elevated-tem- 3(6) mL HCl (38%) 30 s alloys)
perature precipitation heat treatments (artificial 5(10) mL HNO3 (70%) Prepare fresh before use
aging), GP zones may either nucleate metastable 190 mL distilled H2O (concentration
variable)
precipitates or they may dissolve, and metastable Toxic!
precipitates nucleate separately. Cold working 20 mL reagent 7m Ⳮ 80 mL H2O 5–10 s ... 7
subsequent to quenching introduces dislocations B) 2 mL HF (40%) 10–60 s Form thin layer of etching 7
that may serve to nucleate metastable or equilib- 3 mL HCl (38%) Rinse in stream of warm products on the specimen
20 mL HNO3 (70%) water surface
rium precipitates. With prolonged artificial ag- 175 mL distilled H2O
ing, equilibrium precipitates may form. Coarse (Modifed 7m)
equilibrium precipitates form during annealing 8m 0.5–25 g NaOH A few seconds–1 min Al and Al alloys 9
treatments of heat treatable alloy products (O 1 g ZnCl2
temper). They also form during most thermo- 10m 1 drop HF (40%) 20–25 C (70–75 F) Pure Al and Al-Mg, Al-Mg- 9
mechanical treatments prior to solution heat 25(30) mL HCl (38%) 10–60 s Si alloys (etching figures)
treatment. 25(20) mL HNO3 (70%) Toxic!
25(50) mL CH3OH
11m 2 mL HCl (38%) 10 s All kinds of Al alloys 7
Alloying Elements and Impurities 8 mL HNO3 (70%)
45 mL H2O
45 mL CH3OH
Solid solubility of the major alloying elements 12m 10 g NaOH 2 min Grain boundaries, Al-Si, Al- 9
in aluminum as a function of temperature is plot- 5 g K4[Fe(CN)6] Cu alloys
ted in the graph in Fig. 15. Of all the elements, 100 mL distilled H2O
zinc has the greatest solid solubility in alumi- 13m 4 g KMnO4 At ambient temperature, 7– Microsegregation in Al 14
Distilled H2O 45 s alloys
num, with a maximum of 82.8 wt% (66.4 at.%) After dissolution, add 1 g NaOH
listed in Table 5. In addition to zinc, the solid 14m 4 g KMnO4 Specimen surface must be Chemical inhomogeneity and 7
solubilities of silver, magnesium, and lithium are 2 g Na2CO3 well polished and microsegregation in Al
greater than 10 at.% (in order of decreasing max- 94 mL distilled H2O precleaned in 20% H3PO4 alloys
Add a few drops of wetting agent at 95 C (205 F) for
imum solubility). Gallium, germanium, copper, uniform wettability; after
and silicon (in decreasing order) have maximum precleaning, rinse in cold
solubilities of less than 10 at.% but greater than water and immediately
1 at.%. All other elements are less soluble. With immerse in etchant for
the one known exception of tin (which shows a 30 s.
15m A) 5 mL HF At ambient temperature, a A) Phase identification 14
retrograde solid solubility between the melting 95 mL distilled H2O few seconds
point of aluminum and the eutectic temperature, At boiling temperature, add MoO3
228.3 C, or 442.9 F, with a maximum of 0.10% until saturation
at approximately 660 C, or 1220 F), the max- B) 10 mL HF B) Grain boundaries
90 mL distilled H2O revealed
imum solid solubility in aluminum alloys occurs At boiling temperature, add MoO3
at the eutectic, peritectic, or monotectic tem- until saturation
perature. With decreasing temperature, the 16m 2–2.5 g (NH4)MoO4 Ⳮ 10 mL HNO3 20 C (70 F) Phase identification 15
solubility limits decrease. This decrease from ap- After dissolution, add 190 mL ethyl 30–40 s
alcohol (stirring intensively)
preciable concentrations at elevated tempera- 17m 1 g (NH4)MoO4 20 C (70 F), 30 s–3 min Phase identification in Al-Si 16
tures to relatively low concentrations at low tem- 200 mL distilled H2O alloys
peratures is one fundamental characteristic that Add 6 g NH4Cl
provides the basis for substantially increasing 18m 1–2 g (NH4)HF2 20 C (70 F) Phase identification 11, 12
2–3 g Na2MoO4 ⳯ 2H2O 30–60 s
the hardness and strength of aluminum alloys by 5 mL HCl
solution heat treatment and subsequent precipi- 100 mL distilled H2O
tation-aging operations.
(continued)
Iron. Virtually all aluminum alloys contain
some iron that is an impurity remaining after re-

Table 4 (continued) example of how microstructures and macros-

No. Chemical composition Etching mode Purpose or application Ref
tructures can be optimized in foundry operations
by influencing eutectic and hypereutectic struc-
19m Stock solution: 20 C (70 F) Phase identification 17
3 g (NH4)MoO4 30–40 s tures in aluminum-silicon alloys. Strength and
20 mL HNO3 ductility of these alloys, especially those with
20 mL distilled H2O higher silicon, can be substantially improved by
Use reagent: modification of the aluminum-silicon eutectic.
1 p. stock solution Ⳮ 4 p. ethyl alcohol
20m 1.44 g (NH)4NO3 Before use, dilute 1:1 with Phase identification 13 No elements are known that beneficially affect
9.4 mL HNO3 water, 15–30 s both eutectic and hypereutectic phases.
100 mL distilled H2O Modification of hypoeutectic alloys (12%
Add MoO3 in excess Si) is particularly advantageous in sand castings
21m 5 mL HCl 30 s All kinds of Al alloys 7
10 mL H2SO4
and can be effectively achieved through the ad-
85 mL distilled H2O dition of a controlled amount of sodium or stron-
22m 2 g NaOH 2–3 min All kinds of Al alloys 7 tium, which refines the eutectic phase. Modifi-
5 g NaF cation is commonly used for those aluminum
93 mL distilled H2O
23m 5 mL CH3COOH (glacial) 20–30 min All kinds of Al alloys 7
alloys with 5% or more silicon. Figure 16 shows
1 mL HNO3 (70%) alloy 356 before and after modification with so-
94 mL distilled H2O dium. Calcium and antimony additions are also
24m 15.5 mL HNO3 (70%) At ambient temperature, All kinds of Al alloys 7 used. Pseudomodification, in which the fineness
0.5 mL HF (48%) immerse 20–60 s, agitating of the eutectic but not the structure is affected,
3 g CrO3 mildly; second etching in
84 mL distilled H2O Keller’s reagent may may be achieved by control of solidification
(Graff-Sargent reagent) reveal further details of the rates.
microstructure. In hypereutectic aluminum-silicon alloys, re-
25m 200 g CrO3 Pre-etch: 4m, next, 50% All kinds of Al alloys 11 finement of the proeutectic silicon phase by
20 g Na2SO4 HNO3 in water, rinse in
17 mL HCl (35%) water, and immediately put phosphorus additions is essential for casting and
1000 mL H2O in 25m product performance. The coarse primary silicon
26m 200 g CrO3 At ambient temperature, 5– All kinds of Al alloys 11 crystals are harmful in the casting and machining
200 g H2SO4 30 s of hypereutectic silicon alloy compositions, and
50 g NH4HF2
1000 mL H2O the function of phosphorus additions is to refine
27m 1–2 mL HNO3 A few seconds–15 min Al-Mg alloys 17 the primary silicon. Figure 17 shows the micro-
98–99% ethyl alcohol structural differences between refined and unre-
fined structures. Phosphorus also reacts with so-
dium, and probably with strontium and calcium,
fining bauxite and smelting. The eutectic com- predicted by the equilibrium phase diagrams be- to form phosphides that nullify the effects of
position of the aluminum-iron system is 1.8 wt% cause of the long times at high temperatures re- modification additions. Therefore, use low-phos-
Fe, and the maximum solid solubility is 0.05 quired to approach equilibrium. phorus metal when modification is a process ob-
wt% Fe at the eutectic temperature of 655 C Aluminum-silicon alloys that do not contain jective. Trace concentrations as low as 0.0015
(1211 F). Solid solubility of iron in aluminum copper additions are used when good castability through 0.03% P are effective in achieving the
is reduced by other alloying elements, and max- and good corrosion resistance are needed. The refined structure.
imum solid solubility of iron is as low as or binary aluminum-silicon system (Fig. 6) is a Al-Si-Mg Alloys. If high strength and hardness
lower than 0.01 wt% Fe in most structural alu- simple eutectic system with a eutectic compo- are needed, magnesium additions make these al-
minum alloys. The equilibrium constituent sition of 12.6 wt% Si and a maximum solid sol- loys heat treatable. Ternary alloys are strength-
ened by precipitation of metastable precursors to
above the solid solubility limit is Al3Fe (h), al- ubility of 1.65 wt% Si (1.5 at.%) at the eutectic
Mg2Si. The quasi-binary section for Al-Mg2Si is
though other phases may be present. Depending temperature of 577 C (1071 F). In the binary
shown in Fig. 18 (Ref 20) for the Al-Mg-Si sys-
on solidification rate and the presence of other aluminum-silicon system, under the nonequilib-
tem. Some 3xx.x casting alloys contain small ad-
elements such as manganese, metastable con- rium conditions of casting, the volume fraction
ditions of magnesium to render them capable of
stituents may occur, such as FeAl6 with moderate of ␣-Al Ⳮ Si eutectic increases linearly from being age hardened. The Al-Mg-Si system also
quenching and Fe2Al9 with rapid quenching (Ref approximately 0 to 1 as silicon content increases is the basis for the 6xxx alloys containing mag-
18). In most cases, the effects of iron in alumi- from 1 to 12%. In large amounts, silicon im- nesium to provide precipitation hardening. Sol-
num are considered in terms of ternary or quar- proves castability and fluidity. Consequently, it idus and solvus projections of the ternary system
tenary phase diagrams, because some iron is al- is used in 4xxx brazing sheet and in 3xx.x and are shown in Fig. 19 (Ref 21). At low magne-
ways present in aluminum alloys. 4xx.x casting alloys. Alloys with silicon contents sium contents, elemental silicon may be present
Silicon is the other ubiquitous impurity in as low as 2% have been used for casting, but as second-phase particles. As magnesium in-
commercial aluminum alloys. Because iron and silicon content usually is between 5 and 13% or creases, both silicon particles and equilibrium
silicon are common impurities in commercially up to 20% Si in hypereutectic casting alloys. Hy- hexagonal Mg2Si constituents may be present.
pure aluminum, the aluminum corner of the Al- pereutectic alloys (12% Si) are used for engine At higher magnesium contents, only Mg2Si is
Fe-Si ternary system is a subject of interest (Ref blocks, because the primary silicon particles are present. With the addition of copper, a complex
19). The presence of iron greatly reduces the sol- wear resistant. quaternary Al4CuMg5Si4 Q phase can form. A
ubility of silicon in aluminum (Ref 19). At low Metallographic structures of the pure compo- precursor to this quaternary phase strengthens
silicon contents, almost all of the iron is present nents and of several intermediate compositions Al-Cu-Mg-Si alloys.
as Al3Fe. With increasing silicon contents, two are shown in Fig. 6. The intermediate composi- Manganese. The aluminum-manganese sys-
ternary phases appear. A hexagonal ␣ phase tions are mixtures of aluminum containing ap- tem (Fig. 20, Ref 22) is the basis for the oldest
(Al8Fe2Si) and then a monoclinic b phase (of proximately 1% Si in solid solution as the con- aluminum alloys. Manganese is an important al-
apparent stoichiometry noticed Al5FeSi or tinuous phase, with particles of essentially pure loying element in wrought compositions but is
Al9Fe2Si2) form initially by peritectic and at the silicon. Hypereutectic alloys show angular pri- normally considered an impurity in casting com-
end of solidification by eutectic transformations. mary crystals of silicon in eutectic (Fig. 6). The positions and is controlled to low levels in most
Phases in commercial products may not be those use of modifiers and refiners is also an important gravity-cast compositions. Manganese offers no

significant benefits in cast aluminum alloys, but grain size. Because only a limited percentage of and cast 5xx.x non-heat-treatable aluminum al-
some evidence exists that a high volume fraction manganese (up to approximately 1.5%) can be loys, which provide excellent combinations of
of MnAl6 in alloys containing more than 0.5% effectively added to aluminum, manganese is strength and corrosion resistance by solid-solu-
Mn may be beneficial for internal casting sound- used as a major element in only a few alloys. tion strengthening and work hardening. The alu-
ness. Manganese also is used as a minor alloying minum-magnesium phase diagram has a posi-
In the straight aluminum-manganese wrought element. In aluminum-magnesium alloys, man- tively sloping solvus, which is a necessary
alloys (3xxx series), manganese increases ganese acts as a grain refiner and probably hin- condition for a precipitation-hardening system
strength without reduction in corrosion resis- ders the formation of the Al-Fe-Mg-Si phase. In such as aluminum-copper. However, the diffi-
tance. They are the most widely used wrought alloys containing copper, manganese precipitates culty in nucleating the fcc Al3Mg2 precipitates
alloys because of their excellent formability and as Al20Cu2Mn3 dispersoid particles. Effects on in the aluminum-magnesium system has pre-
resistance to corrosion. During solidification of strength are minor, but the dispersoids aid in cluded commercialization of heat treatable alu-
commercial-sized ingots, some of the manganese grain size control after solution heat treatment. minum-magnesium alloys, unless they contain
forms initially orthorhombic Al6(FeMn) by eu- In silicon alloys, manganese counteracts the enough silicon, copper, or zinc to form Mg2Si,
tectic reaction, then cubic Al15(FeMn)3Si2 by damaging effects of high iron content in alumi- Al2CuMg or Al2Mg3Zn3 precipitates. Binary
peritectic, and in the residual liquid by eutectic num-silicon alloys by the formation of ␣- aluminum-magnesium alloys are widely used in
transformations. The remaining manganese re- Al15(FeMn)3Si2 phase (in form of Chinese applications requiring a bright surface finish and
mains in solution and is precipitated during script) at the expense of b-Al9Fe2Si2 (in form of corrosion resistance, as well as attractive com-
the ingot preheat as ␣-Al15(FeMn)3Si2 or sharp needles). binations of strength and ductility. Common
Al6(Mn,Fe) dispersoids. These dispersoids Magnesium. The aluminum-magnesium sys- compositions range from 4 to 10% Mg, and com-
strengthen the material and control recrystallized tem (Fig. 21) is the basis for the wrought 5xxx positions containing more than 7% Mg are heat
Fig. 5 Examples of dispersed precipitates shown at various magnifications. (a) Transmission electron microscopy image (at 200,000⳯) of g⬘ phase in thin foil of 7050-T6 alloy. (b)
Micrograph (at 1000⳯) of heat treated (T6) 418 alloy etched with 0.5% HF (etchant 5m in Table 4). (c) Micrograph (at 400⳯) of heat treated 7050-T6 alloy etched with 0.5%
HF (etchant 5m in Table 4)

treatable. Instability and room-temperature ag- Zinc. This element confers little solid-solu- not necessary for optimal properties in most Al-
ing characteristics at higher magnesium concen- tion strengthening or work hardening to alumi- Zn-Mg alloy castings. However, microsegrega-
trations encourage heat treatment. num. No significant technical benefits are ob- tion of magnesium-zinc phases can occur in
Alloys in the 6xxx series contain silicon and tained by the addition of just zinc to aluminum, these alloys, which reverses the accepted rule
magnesium in the approximate proportions re- but the addition of copper and/or magnesium that faster solidification results in higher as-cast
quired for formation of magnesium silicide with zinc results in attractive compositions for properties. When it is found in an Al-Zn-Mg al-
(Mg2Si), thus making them heat treatable. Al- heat treating or natural aging. Usually, other ele- loy casting that the strength of the thin or highly
though not as strong as most 2xxx and 7xxx al- ments, such as chromium, are also added in chilled sections are lower than the thick or
loys, 6xxx-series alloys have good formability, small quantities. slowly cooled sections, the weaker sections can
weldability, machinability, and corrosion resis- The Al-Zn-Mg precipitates provide the basis be strengthened to the required level by solution
tance, with medium strength. Magnesium also is for the 7xxx wrought alloys and the 7xx.x cast heat treatment and quenching, followed by nat-
the basis for strength and hardness development alloys. Two phases can form by eutectic decom- ural or artificial (furnace) aging.
in heat treated aluminum-silicon alloys and is position in commercial Al-Zn-Mg alloys: hex- Chromium. In commercial alloys, the solu-
commonly used for the same purpose in more agonal MgZn2 and body-centered cubic bility can be reduced to such an extent that Al7Cr
complex aluminum-silicon alloys containing Al2Mg3Zn3. Depending on the zinc/magnesium primary particles can form by a peritectic reac-
copper, nickel, and other elements. The harden- ratio, copper-free alloys are strengthened by tion at chromium contents lower than that indi-
ing phase of Mg2Si displays a useful solubility metastable precursors to either MgZn2 or cated by the binary aluminum-chromium phase
limit corresponding to approximately 0.70% Al2Mg3Zn3. In Al-Zn-Mg-Cu alloys, copper and diagram. Because coarse primary particles are
Mg, beyond which either no further strengthen- aluminum substitute for zinc in MgZn2 to form harmful to ductility, fatigue, and fracture tough-
ing occurs or matrix softening takes place. Com- Mg(Zn,Cu,Al)2. Particles of Al2CuMg can also ness, the upper limits of chromium depend on
mon premium-strength casting compositions in form in these alloys by eutectic decomposition the amount and nature of the other alloying and
the aluminum-silicon family employ magnesium and solid-state precipitation. Figure 22 shows impurity elements. In 5xxx alloys, fcc cubic
in the range of 0.40 to 0.070%. solid solubilities of various phases in the alu- Al18Mg3Cr2 dispersoids precipitate during ingot
Copper. The aluminum-copper system is the minum corner. preheating. In 7xxx alloys, the composition of the
basis for the wrought 2xxx and cast 2xx.x alloys, The high-temperature solution heat treatment dispersoids is closer to Al12Mg2Cr. Chromium
and many other heat treatable alloys contain cop- and drastic quenching required by other alloys dispersoids contribute to strength in non-heat-
per. Alloys containing 4 to 6% Cu respond most (Al-Cu and Al-Si-Mg alloys, for example) are treatable alloys and control grain size and degree
strongly to thermal treatment. Heat treatable alu-
minum-copper alloys can reach quite high
strengths with good ductility, especially if pre-
pared from ingot containing less than 0.15% Fe. Table 5 Solubility limits of various binary aluminum alloys
In commercial aluminum-copper alloys, some of Temperature(a) Liquid solubility Solid solubility
the copper chemically combines with aluminum Element C F wt% at.% wt% at.%
and iron to form either tetragonal Al7Cu2Fe or Ag 570 1060 72.0 60.9 55.6 23.8
orthorhombic ␣(Al,Cu,Fe) constituent particles Au 640 1180 5 0.7 0.36 0.049
during solidification. These constituents cannot B 660 1220 0.022 0.054 0.001 0.002
be dissolved during subsequent thermal treat- Be 645 1190 0.87 2.56 0.063 0.188
Bi 660(b) 1220(b) 3.4 0.45 0.1 0.01
ments, but one can transform to the other during Ca 620 1150 7.6 5.25 0.1 0.05
thermal treatments of ingots or castings. During Cd 650(b) 1200(b) 6.7 1.69 0.47 0.11
heat treatment of aluminum-copper alloys con- Co 660 1220 1.0 0.46 0.02 0.01
taining little magnesium, Al2Cu precipitates as Cr 660(c) 1220(c) 0.41 0.21 0.77 0.40
Cu 550 1020 33.15 17.39 5.67 2.48
the strengthening phase. Fe 655 1210 1.87 0.91 0.052 0.025
Adding magnesium to aluminum-rich alumi- Ga 30 80 98.9 97.2 20.0 8.82
num-copper alloys results in the formation of the Gd 640 1180 11.5 2.18 0.1 0.01
Al2CuMg phase by eutectic decomposition. Ge 425 800 53.0 29.5 6.0 2.30
Hf 660(c) 1220(c) 0.49 0.074 1.22 0.186
Metastable precursors to face-centered ortho- In 640 1180 17.5 4.65 0.17 0.04
rhombic Al2CuMg precipitates are used to Li 600 1110 9.9 30.0 4.0 13.9
strengthen several structural alloys used in the Mg 450 840 35.0 37.34 14.9 16.26
aerospace industry, because they confer a desir- Mn 660 1220 1.95 0.97 1.25 0.62
Mo 660(c) 1220(c) 0.1 0.03 0.25 0.056
able combination of strength, fracture toughness, Na 660(b) 1220(b) 0.18 0.21 0.003 0.003
and resistance to the growth of fatigue cracks. Nb 660(c) 1220(c) 0.01 0.003 0.22 0.064
Al-Cu-Si Casting Alloys. Aluminum-copper Ni 640 1180 6.12 2.91 0.05 0.023
alloys with somewhat higher copper contents (7 Pb 660 1220 1.52 0.20 0.15 0.02
Pd 615 1140 24.2 7.5 0.1 0.02
to 8%), formerly the most commonly used alu- Rh 660 1220 1.09 0.29 0.1 0.02
minum casting alloys, have steadily been re- Ru 660 1220 0.69 0.185 0.1 0.02
placed by Al-Si-Cu/Mg (3xx.x) alloys. Alumi- Sb 660 1220 1.1 0.25 0.1 0.02
num-copper-silicon alloys are the most widely Sc 660 1220 0.52 0.31 0.38 0.23
Si 580 1080 12.6 12.16 1.65 1.59
used aluminum casting alloys. The amounts of Sn 230 450 99.5 97.83 0.01 0.002
both additions vary widely, so that the copper Sr 655 1210 ... ... ... ...
predominates in some alloys and the silicon in Th 635 1180 25.0 3.73 0.1 0.01
others. In these alloys, the copper contributes to Ti 665(c) 1230(c) 0.15 0.084 1.00 0.57
Tm 645 1190 10.0 1.74 0.1 0.01
strength, and the silicon improves castability and U 640 1180 13.0 1.67 0.1 0.01
reduces hot shortness. Aluminum-copper-silicon V 665(c) 1230(c) 0.25 0.133 0.6 0.32
alloys with more than 3 to 4% Cu are heat treat- Y 645 1190 7.7 2.47 0.1 0.03
able, but usually heat treatment is used only with Zn 380 720 95.0 88.7 82.8 66.4
Zr 660(c) 1220(c) 0.11 0.033 0.28 0.085
those alloys that also contain magnesium, which
enhances their response to heat treatment. (a) Eutectic reactions unless designated otherwise. (b) Monotectic reaction. (c) Peritectic reaction. Source: Ref 3, 4

of recrystallization in heat treatable alloy prod- 1960s contain small amounts of zirconium, usu- Cu-Li phases. Because of its high cost relative
ucts. ally less than 0.15%, to form Al3Zr dispersoids to other alloying elements, lithium alloys have
Zirconium also forms a peritectic with alu- for recrystallization control. been found to be cost-effective thus far only in
minum. The phase diagram predicts that the Lithium. This element reduces the density and space and military applications.
equilibrium Al3Zr phase is tetragonal, but fine increases the modulus of aluminum alloys. In Tin. Aluminum-tin alloys that contain approx-
dispersoids of metastable cubic Al3Zr form dur- binary alloys, it forms metastable Al3Li precip- imately 6% Sn (and small amounts of copper and
ing ingot preheating treatments. Most 7xxx and itates and combines with aluminum and copper nickel for strengthening) are used for cast bear-
some 6xxx and 5xxx alloys developed since the in Al-Cu-Li alloys to form a large number of Al- ings because of the excellent lubricity imparted
Fig. 6 Aluminum-silicon phase diagram and cast microstructures of hypoeutectic compositions (12% Si), hypereutectic compositions (12% Si), and one close to the eutectic
composition of 12% Si
Fig. 7 Networklike morphology of second-phase structure in two hypoeutectic alloys. (a) As-cast 356 alloy. (b) As-cast 7050 alloy. Both etched with 0.5% HF (5m in Table 4) and
magnified by 100⳯

by tin. These tin-containing alloys were devel- formation anisotropy, inclusions distribution), the presence of some defects (scratches, bubbles,
oped for bearing applications. and grain-flow patterns. Macroscopic examina- inclusions, cracks, and deposit extruded section).
tion can also reveal various features in castings, In all cases, the results of a macroexamination
such as: can be influenced by the conditions of observa-
Examination of tion and especially by the strength and orienta-
● Casting discontinuities, such as shrinkage,
Macrostructure (Ref 1, 8, 9, 23–25) gas pores, and freezing cracks
tion of the illumination relative to the specimen
surface and the observer. Specimen rotation rela-
● Grain size and its morphology and distribu-
Examination of macrostructure is done at low tive to the lighting source is very often used to
tion, dendrite morphology and dispersion de-
magnification of approximately 10⳯ or less. reveal the true macrostructure image and to ob-
gree, and results of the cooling-rate changes
Macroscopic examination is usually a prelimi- tain satisfactory results. However, the light re-
on the primary cast part structure morphology
nary procedure prior to microstructural exami- flection from some planes of the examined sur-
● Chemical or structural heterogeneity of cast
nation. In addition, macroscopic examination is faces can sometimes be incorrectly interpreted.
material
often used in the inspection and quality control Thus, macroscopic observation (and photogra-
● Segregation of the contaminants and inclu-
of finished or semi-finished products such as phy for purposes of documentation) demands
sions during alloy solidification
castings, wrought forms, and welds. In wrought some skill.
forms, macroscopic examination can help iden- Macrostructure can be examined from a part Of course, macroscopic observation of frac-
tify, for example, discontinuities (such as surface, a fracture surface, or a prepared macro- ture surfaces is also an important and useful step
cracks), inhomogeneous features (such as de- section. Examination of a part surface can reveal in failure analysis. Several kinds of surface
Fig. 8 Dispersed phase and networklike morphology of second-phase structure in two eutectic alloys. (a) As-cast 413 alloy at 750⳯. (b) As-cast aluminum-copper alloy at 400⳯.
Both etched with 0.5% HF (5m in Table 4)
Fig. 9 Dispersed phase and networklike morphology of second-phase structure in two hypereutectic alloys. (a) As-cast 390 alloy with primary precipitates of silicon (light gray). (b)
As-cast 384.0 alloy with primary precipitates of Al-Fe-Si. Both etched with 0.5% HF (5m in Table 4) and magnified by 100⳯

markings or topological features may help iden- ration other than cleaning and degreasing the regard to the same general rules for preparation
tify the crack origin and the mechanism of crack sample. However, care of evidence is a critical of specimens for microstructural examination.
propagation. Other features that may be visible factor in failure analysis investigations, and the The relatively soft matrix makes the specimen
on a fracture surface include: method demands skill from the investigator, be- very susceptible to superficial deformation. In
cause the objective criteria of the result interpre- such case, the grain and dendrite morphology
tation are not established or not repeatable in can be distorted. Discontinuities such as shrink-
● Different kinds of inclusions
many cases. Lightening is also important, espe- age, gas porosity, and cracks also can be
● Porosity, shrinkage, and other discontinuities
cially when in the photography of fracture sur- smoothed or deformed, thus making it impossi-
● Grain size heterogeneity
faces (e.g., see the article “Photography in Fail- ble to reveal these defects by dye penetrants or
● Zones of solidification
ure Analysis” in Failure Analysis and other aids. A machined surface of the specimen
● Overheating (eutectic melting)
Prevention, Volume 11 of ASM Handbook, can be acceptable for macroscopic etching. Nev-
● Oxide stringers
2002). ertheless, the tools used for cutting and machin-
● Bright and dark flakes
Preparation and Examination of Macrosec- ing should be sharp with a suitable choice of feed
tions (Ref 1, 2, 8, 9, 25). Preparation proce- and adjustment to a favorable cutting speed. A
Visual or low-magnification examination of a dures (cutting and machining) of aluminium-al- shaper or milling machine is preferred for secur-
fracture surface does not involve special prepa- loy macrosections should be carried out with ing the constant cutting speed.
Fig. 10 As-cast morphologies in a eutectic aluminum-silicon alloy. (a) Unmodified alloy with coarse silicon precipitates formed during solidification. (b) Modified alloy with
solidification of finer silicon precipitates. Both etched with 0.5% HF (5m in Table 4) and magnified by 750⳯
Fig. 11 Effect of heat treatment on phase morphology in a hypoeutectic alloy (alloy 355). (a) As-cast structure (at 500⳯ magnification) with a continuous network of interdendritic
precipitates of eutectic silicon. (b) Heat treated condition (T6) of same alloy with globular eutectic silicon precipitates shown at 750⳯. Both etched with 0.5% HF (5m in
Table 4)

Fig. 12 Effect of heat treatment on phase morphology in alloy 7050. (a) As-cast structure with network of Al Ⳮ M(MgZn2) eutectic and Al2Mg3Zn3(T) precipitates. (b) Heat treated
(T6) condition with globular morphology of M(MgZn2) eutectic and Al2Mg3Zn3(T) precipitates. Both etched with 0.5% HF (5m in Table 4) and magnified by 500⳯
The preliminary preparation of the specimen ment of the laboratory. Some reagents (e.g., HF) 1. Preparation of specimens with a flat and
surface is important. Smoother specimen sur- should be stored in special containers made of smooth surface
faces without deformation allow better exami- materials that are resistant to reaction with their 2. Intensification of contrast between phase or
nation of details and good repeatability of results contents. structure constituents
after macroetching. The risk of loss of the some 3. Microscopic observation
structure details during intensive and/or pro- 4. Description and interpretation of the observed
longed macroetching (to remove the initial Examination of Microstructure microstructure
surface roughness) can be avoided by good pre- (Ref 1–6, 8–17, 23, 25–40) The first step is specimen preparation, which
liminary preparation. Degreasing or special pre-
consists of several processes to obtain microsec-
cleaning of the specimen surface is not necessary
Microscopic examination is carried out on tions with smooth, mirrorlike surfaces. This is
but can be helpful for obtaining uniform and
metallographic microsections with prepared sur- followed by various techniques to enhance con-
clear results of revealing the macrostructure. The
faces. The process involves four basic steps: trast between structure or phase constituents.
best degreaser is a caustic reagent (Table 6). Its
use is recommended before porosity observation
on macrosections. In case of unclear results, the
surface can be slightly rubbed with a pencil
eraser to improve the contrast. A light pre-etch-
ing with a caustic reagent before the dye pene-
trant application removes some sealing of the po-
rosity by smeared metal. The etching of the
macrosections reveals the details of the structure,
enabling an observation and description of its
features (Table 7).
The following effects of the macroetching
procedure should be observed:
● Surface smoothing
● Structure defects revealed: cracks, porosity,
superficial defects, intergranular corrosion
● Structure features revealed: macrosegrega-
tion, grain size, rolling direction, welding
zone
Reagents used for macroetching are very con-
centrated and have a strong action. Special pre-
cautions that are recommended for handling and
storage should be followed. Cooling ventilation
(in case of the effects of an exothermic reaction
with a sample or during the mixing of the com-
ponents) is necessary because many of the com-
ponents, as concentrated acid vapors, are volatile
and can irritate the respiratory tract. Gloves,
glasses, and aprons should be the default equip- Fig. 13 Aluminum-chromium phase diagram illustrating the peritectic reaction

Fig. 14 Micrographs of peritectic structures. (a) Al-Fe-Mn-Si alloy (at 200⳯) with primary phase of Al3Fe(Mn) and peritectic phase of ␣-AlFeMnSi. (b) Al-Fe-Cu-Ni alloy (at 400⳯)
with Al3Ni primary phase and an Al9FeNi peritectic phase. Both etched with 0.5% HF
The initial preparation involves cutting of spec- material is eliminated during the next stage of Another important problem is the choice of
imens, mounting, and smoothing of the surface. preparation. the zone in obtaining a representative material
The hard phase constituents need the higher specimen of the manufactured part. In the case
load and longer cutting time that increase the risk of morphological anisotropy of the microstruc-
Specimen Cutting of fracture or pullout of certain microstructure ture (especially in the wrought alloys), the mi-
constituents and the embedding of its parts into crosection plane should be oriented in relation to
The following properties of aluminum alloys
the matrix, making a false image of the micro- the rolling direction (parallel or perpendicular).
should be taken into account at the specimen cut-
structure and creating additional problems dur-
ting stage:
ing the next specimen preparation steps.
● The softness and ductility of the aluminum Dispersion-strengthened material is much Mounting (Ref 1, 6)
solid-solution (␣) matrix harder than the pure aluminum matrix. A tem-
● The presence of a hard and brittle microstruc- perature comparable with the temperature of the Usually, the examined specimen is mounted
ture component—as silicon in the cast alloys structure process in the solid state (precipitation, in a thermoset plastic material (e.g., Bakelite,
or as intermetallic phases in both cast and solid-solution decomposition, recovery, and re- duracryl) hardened under temperature or chem-
wrought alloys in either the rough or treated crystallization) can be easily achieved during the ical action. Specimens are mounted in resin to
state (Table 2) cutting operation (Table 8). From this point of make the preparation easier or faster (in the case
● The low temperature of the phase transfor- view, the most appropriate method of sample of using an automated grinding-polishing ma-
mation in the solid state (Table 8) and the sectioning is abrasive wet cutting. chine). Specimen mounting is also necessary for
disperse precipitation during heating of the
particle-hardened alloys
During cutting of the specimen, deformation
of the alloy matrix can be introduced, which is
very important. For this reason, the cut plane
should be situated as far as possible from the
examined region. This assures that the deformed
Fig. 16 Effect of sodium modification on microstructure of sand-cast aluminum-silicon hypoeutectic alloy 356-F. Both
specimens were etched in 0.5% hydrofluoric acid and are shown at 100⳯. (a) As-cast structure in unmodified
alloy consists of a network of silicon particles (sharp gray), which formed in the interdendritic aluminum-silicon eutectic.
Fig. 15 Equilibrium binary solid solubility for common (b) Modified alloy by addition of 0.025% Na to the melt. Constituents are the same as in (a), but the particles of silicon
alloying elements of aluminum are smaller and less angular

edge retention with samples of fracture profiles, standard available materials for sample mount- ● No introduction of foreign particles
coating layers, perpendicular cross sections of ing can be divided into two groups: ● Retained, flat edges
very thin samples (such as rolled sheet, foils, and ● No thermal modification of the microstruc-
● Hot-mounting resins
wire ends), and materials with surface inhomo- ture
● Cold-mounting resins
geneity. Mounting is also necessary when dis-
continuities involve material porosity or internal Although hot-mounting resins are less expen- Grinding (Ref 1, 6). The main aims of grind-
cracks. The mounting of the specimen also fa- sive, a mounting press is required for their use. ing are:
cilitates handling and allows for more consistent They cure at elevated temperature (even as high ● To remove material deformed during cutting
planeness between the opposite sides of the spec- as 180 C, or 355 F), which could be inadvisable (rough, plane grinding)
imen. This is important when performing micro- for aluminum alloys. However, some hot-mount- ● To remove the superficial layer of the speci-
hardness measurements. ing resins are conducting resins, which may be men that covers the material destined for ex-
Specimen cleaning (with organic solvents in very useful when samples are intended for scan- amination (rough, plane grinding)
an ultrasonic cleaner) is recommended before ning elctron microscopy (SEM) examination and ● To prepare a flat surface while introducing
embedding into resin to guarantee a good adhe- x-ray microanalysis. Nevertheless, for aluminum only some residual or superficial deformation
sion of the resin to the specimen surface. The alloys, the cold-mounting resins should be rec- that can be eliminated during polishing (fine
ommended. Vacuum impregnation of the porous grinding)
materials (porosity is a very frequent defect of
cast parts) can be used to improve the filling of For relatively soft materials such as aluminum
internal pores and for revealing their micropro- alloys, the most useful abrasive for grinding is
file. silicon carbide. Commercial papers with rela-
tively coarse SiC abrasive particles are used for
rough grinding. Abrasive papers with gradations
Specimen Smoothing (Ref 1, 6) of SiC particles are used in subsequent steps for
fine grinding with reduced SiC particle size.
Specimens with a flat, mirrorlike surface on a With a typical automated grinding-polishing
microscopic scale are prepared by various grind- machine, the grinding operation can be divided
ing and polishing procedures. Mechanical abra- into two steps:
sion is the most common method of smoothing
and polishing the surface of a metallographic mi- ● Rough grinding (for planeness) with the com-
crosection so that the specimen is suitable for mercial SiC wet grinding papers of decreas-
examination at high magnification with the small ing grain size, starting from 120-grit paper,
depth of field of a light microscope. When the with water lubricant
polished microsection is properly prepared, the ● Fine grinding (to remove scratches from pre-
high-quality surface should be devoid of imper- vious paper gradation) with commercial SiC
fections such as those shown in Fig. 23 and 24. wet grinding papers, starting from 500-grit
The objectives of a properly polished specimen paper, with water lubricant
are:
The loading and time of process should be es-
● No deformation from cutting tablished individually, depending on the initial
● No scratches from grinding or polishing state of the samples. A typical procedure for the
● No pullouts of the brittle structure constitu- recommended fine grinding of aluminum alloys
ents is shown in Table 9.
Fig. 17 Effect of phosphorus refinement on the micro-

structure of Al-22Si-1Ni-1Cu alloy. (a) Unrefi-
ned. (b) Phosphorus-refined. (c) Refined and fluxed. All Fig. 18 Quasi-binary section showing the solid solubility of Mg2Si in aluminum for the Al-Mg-Si ternary. Source:
100⳯ Ref 20

Solubility limits, wt%, at:

559 C 550 C 500 C 400 C 200 C
Constituent (1038 F) (1022 F) (932 F) (752 F) (392 F)
Mg 0.68 0.66 0.54 0.28 0.05
Si 1.16 1.04 0.60 0.24 0.04
Fig. 19 Al-Mg-Si ternary diagrams. (a) Solidus projection. (b) Solvus projection. Solid-solubility limits along the locus for the aluminum-rich apex of the (Al) Ⳮ Mg2Si Ⳮ (Si) phase
field are given in the table. Source: Ref 21
Recently designed grinding-polishing ma- Diamond polishing is the fastest way to obtain form of polycrystalline sprays, suspensions, and
chines also feature magnetic platens for quick a flat specimen surface without scratches and ar- paste. The optimal polishing results are achieved
substitution of steel-backed grinding papers. The tifacts. Because of its very high hardness, dia- when the homogeneity of the grain size and the
use of magnetic discs and steel-backed paper/ mond is able to cut almost all phase constituents shape of the diamond particle are controlled. The
cloth reduces time in the removal and replace- of the aluminum alloys. The diamond materials following gradations of diamond abrasives are
ment of worn grinding paper. When automated for metallographic microsections are used in the recommended: 3, 1, and 0.25 lm, successively.
grinding-polishing machines are used in smooth-
ing mounted or unmounted specimens, holders
are also needed to maintain planeness and the
flat surface of the specimens. Various commer-
cial holders are available, depending on the
needs. Sometimes, the holders can be adjusted
for the different mechanical preparation steps
without removal from the machine and can be
equipped with special clamps (for small-wire
ends, plates, or untypical-shaped specimens).
Polishing (Ref 1, 6). The two most common
methods for polishing metallographic microsec-
tions are by mechanical or electrochemical
means. The main objective of polishing is to re-
move material deformation introduced by pre-
vious grinding and to obtain a flat, mirrorlike
surface on a microscopic scale.
Mechanical Polishing. Table 10 lists a typical
procedure recommended for the polishing of alu-
minum alloys. During successive steps of me-
chanical polishing, finer and finer abrasive par-
ticles are used. Two main groups of abrasive
materials are usually used for polishing alumi-
num alloys:
● Diamond abrasive
● Oxide abrasive materials Fig. 20 Aluminum corner of aluminum-manganese phase diagram. Adapted from Ref 20 and 22

Aluminum alloys characterized by a soft and ● Chemical, physical, and electrochemical These methods enhance contrast and improve
ductile matrix can often require final polishing. treatments of the metallographic microsection microscopic observation of phases, as shown in
Good results are obtained by using oxide-abra- the examples in Fig. 25 and 26. Most metallo-
Contrast enhancement is also achieved in
sive media. Colloidal dispersions of silica (SiO2) graphic light microscopes are equipped with a
scanning electron microscopy by detection of
particles with 0.04 lm particle size are used for cross-poles mode of observation, where two Ni-
secondary electrons (typical topographic con-
final polishing to produce aluminum alloy mi- col prisms are used as polarizer and analyzer.
trast of a SEM) or by detection of back-scattered
crosections without any scratches, deformation, Their mutual rotation allows the choice of the
electrons (composition and topographic con-
or surface artifacts. Because of its low alkalinity optimal position to reveal some phase constitu-
trast).
(pH 9.8), this polishing medium also can simul- ents or differentiate the contrast between some
Illumination with a Light Microscope. Il-
taneously act as an etchant, especially in the case microregions, such as the grains or dendrites of
lumination of the specimen with a light micro-
of grain boundaries and some intermetallic an anisotropic material.
scope can be done with:
phases present in aluminum alloys. The polish- Chemical and Physical Treatments of the
ing is carried out by using special polishing ● Polarized light Metallographic Microsection. Contrast be-
cloths wet with lubricants. A water-free diamond ● Phase contrast, Nomarski contrast tween phases or microstructural constituents of
suspension or spray with a carefully controlled ● Bright or dark field a polished microsection can be improved by ad-
narrow range of diamond particle grain size and
shape is used to ensure a high level of reproduc-
ibility.
Electrolytic polishing can be a fast and clear
way to reveal microstructural features without
introducing any superficial deformation and
changes in the material caused by local heating
during mechanical treatment (Ref 1, 23, 25).
Nevertheless, this procedure needs special re-
agents (Table 11) and equipment. A variable
shape and size of the specimen is acceptable with
this method. The main principle is that a speci-
men is an anode in an electrochemical cell,
where the conditions of the process are adjusted
to uniformly dissolve the superficial layer of the
specimen material. This is very difficult to reach
in the case of a polyphase material. The follow-
ing are negative aspects of this method for alu-
minum alloys:
● The quality (flat and uniform) of the polished
surface may be susceptibile to chemical and
structural inhomogeneities of the alloy.
● Continuous and precise control of the current
density or voltage conditions is needed, de-
pending on the chemical composition and
structural state of the alloy.
● Local electrochemical cell formation (inter- Fig. 21 Aluminum end of the the aluminum-magnesium phase diagram. Adapted from Ref 18 and 20
face dissolution) (e.g., Table 12) may cause
the intermetallic inclusion to crumble away.
A material containing numerous nonmetallic in-
clusions (aluminum oxides) should be polished
mechanically with special precaution.
Chemical polishing reagents (Table 13) some-
times are used. Chemical polishing is rather rare,
because continual improvements have made me-
chanical polishing more effective and easier. Me-
chanical methods are also less toxic.
Contrast Enhancement of
Phases (Ref 1, 5, 6, 8–17, 23, 25, 26)
Most of the phase constituents are visible after
the fine-polishing step, but very often, the visible
contrast under a microscope is too light either to
identify the phases or to measure their stereolog-
ical parameters. Two main techniques for im-
proving contrast to reveal constituents in light
microscopy are:
● Special illumination of the microsection dur-
ing microscopic observation Fig. 22 Aluminum corner of the Al-Mg-Zn system showing solid solubilities of various phases. Source: Ref 20

ditional surface treatments. This includes chem- croscopes used in metallography. The choice of degree of dispersion. As noted, specimens
ical or electrochemical etching and physical sur- a microscopic technique depends on the required should be examined immediately after prepara-
face treatments that deposit an interference layer resolution, the methods of specimen preparation, tion because of the very fast surface oxidation of
on the specimen. and the microstructural constituents in terms of aluminum alloys. This is especially important
Chemical and Electrochemical Etching. Elec- their chemical composition, morphology, and with SEM or x-ray microanalysis. In transmis-
trochemical and chemical reagents for etching
aluminum alloys are shown in Tables 14 and 15,
respectively. The three main objectives of etch-
ing are: Table 6 Reagents for chemical macroetching
No. of reagent Chemical composition(a) Etching mode Purpose or application Ref
● Attack and reveal the grain boundaries and
1M caustic 100 mL distilled H2O 5–15 min Commercial Al and Al alloys 9
the interface regions between the matrix and etchant 10–20 g NaOH 60–70 C (140–160 F)
phase constituents 90 mL distilled H2O 5–15 min 7
● Cover selected phase constituent surface with 10 g NaOH 60–70 C (140–160 F)
a thin film of chemical reaction products that Rinse in water, then clean by fast
dip in 50% HNO3
improve or reveal contrast between different 2M 75 mL HCl, (38%) Seconds to minutes Cast Al-Si alloys, Al-Cu, Al- 9
structure components (visible in black-and- 25 mL HNO3, (70%) Use freshly prepared reagent; Mn, Al-Mg, Al-Ti
white mode) 5 mL HF, (40%) rinse specimen with warm
● Cover selected phase areas with a thin film of (Ⳮ25 mL distilled H2O) water
3M Flick’s 90 mL distilled H2O 5 s–3 min Pure Al, wrought parts 9
chemical reaction products that die/color the reagent 15 mL HCl
phase in a specific manner to allow phase 10 mL HF, (40%)
identification (visible in a color mode) 4M Keller’s 20(50) mL distilled H2O 1–3 min All kinds of Al alloys; 9
reagent 20(25) mL HNO3, (70%) reveals grain size, rolling
The micrographs in Fig. 27 and 28 are ex- 20(15) mL HCl, (38%) direction, welding zone
5(10) mL HF, 40%
amples of etching effects to reveal grain bound- 5M Tucker’s 25 mL distilled H2O Seconds to minutes Pure Al 9
aries and phase boundaries, respectively. Etchant reagent 45 mL HCl, (38%) Use freshly prepared reagent
effect in revealing phase constituents is shown 15 mL HNO3, (70%)
in Fig. 29. Both chemical and electrolytic etch- 15 mL HF, 40%
27 mL distilled H2O (warm) 6 min Higher HNO3 concentration 8
ing achieve best results when freshly polished 16 mL HNO3, (70%) can improve contrast
specimens are etched, because aluminum and its 42 mL HCl, (38%)
alloys tend to be covered with passivating oxide 15 mL HF, (40%)
film. If necessary, the specimen surface should 25 mL distilled H2O Freshly prepared before using. ... 7
45 mL HCl, (38%) Etching time until desired
be degreased before etching. Sometimes, suc- 15 mL HNO3, (70%) result is observed; repeat every
cessive polishing and etching are repeated for 15 mL HF, (48%) 10–15 s; rinse in warm water
best results. 6M 100 mL distilled H2O Seconds to minutes Superficial defects of pure Al 9
Applications of the various chemical etchants 5.5 mL H2SO4, (98%)
7M Dix-Keller’s 950 mL distilled H2O 5–20 s at ambient temp. Rinse Al-Zn-Mg-Cu. Grains are 8
are listed in Table 15. Electrolytic etching, which reagent 25 mL HNO3, (70%) with warm water, next with tinted depending on crystal
is often called an anodic oxidation (because the 15 mL HCl, 1.19 (38%) alcohol orientation
specimen is an anode), is especially useful for 10 mL HF, 40%
deformed and recrystallized wrought alloy as 8M 9 g H3PO4 30 min at ambient temp. Reveals intergranular 8
100 mL distilled H2O corrosion and flow lines in
well. During etching, the grain boundaries are Al-Mg alloys
attacked and the grains covered with the oxide 9M Zeerleder’s 10 g FeCl3 At ambient temperature, time Pure Al 8
layer. The specimen observed in polarized light reagent 100 mL distilled H2O according to observation
reveals the grain structure and their crystallo- 0.5 mL HF, 40%
10M Poulton’s 12 mL HCl, (38%) May be prepared and stored. All kinds of Al alloys 7
graphic orientation; that is, the grains of the dif- reagent 6 mL HNO3, (70%) Avoid both specimen and
ferent crystal orientation have the different color. 1 mL HF, (48%) reagent heating during etching;
Physical Deposition of Interference Layer 1 mL H2O rinse in cold water
(Ref 16, 25). Microstructural phases can be re- 11M 1 mL HF, (48%) Used on prepared surfaces. Time All kinds of Al alloys 7
9 mL distilled H2O of immersion until expected
vealed by covering the specimen surface with the effect is observed; rinse in hot
interference layer formed during vacuum depo- water
sition of the evaporated (sublimated) or sput- 12M 50 mL HCl Prepare fresh before using. 10–15 All kinds of Al alloys 7
tered medium. The resultant color contrast is 15 mL HNO3, (70%) C (50–60 F). In cold water
3 mL HF, (8%) bath, time of immersion until
very dependent on the interference layer thick- 5 mL FeCl3 (conc. solution) expected effect is observed
ness. A very thin layer absorbs all the wave- 13M 60 mL HCl Prepare fresh before using. All kinds of Al alloys 7
lengths and gives a gray contrast. If a thicker 40 mL HNO3 (70%) Immerse for a few seconds,
layer is applied, selective interference of one repeat until expected effect is
observed
wavelength and the intensification of another 14M 20 g CuCl2 Etching time a few seconds; All kinds of Al alloys 7
causes the color contrast to appear. These meth- 100 mL H2O repeat until expected result is
ods can be used for phase identification only observed, cleaning each time
when strict control of the interference layer in cleaning mixture:
6 p. HNO3 (70%)
thickness is possible. 1 p. HF
Rinse in water between steps
15M 10 mL HCl Mix before use; add HCl last. At All kinds of Al alloys 7
Observation and 30 mL HNO3 (70%) ambient temp., immerse a few
Description of Microstructure 20 mL H2O seconds, rinse in cold water,
5 g FeCl3 repeat until desired effect is
observed
Table 16 summarizes the observation charac-
teristics for the three most common types of mi- (a) Always add an acid into water.

sion electron microscopy (TEM), specially pre- of the specimen and chemical composition of the analysis can be necessary. Detection of back-
pared specimens (thin foils or replicas) are re- phase constituents on the results. Their apparent scattered electrons in a SEM is a very useful but
quired. Interpretation of the contrast from thin stoichiometry is usually established on the basis seldom used method. This method provides an-
foils under a TEM is difficult and related to the of the average chemical composition. The range other alternative when phase attribution by mor-
local crystal structure of the material. of possible composition is rather wide; some- phology, color, and/or chemical composition is
Interpretation of microstructural images re- times, an array of the continuous solid solutions not successful. This last method allows the crys-
quires the attribution of microstructural features may exist between two equilibrium systems (Al- tal structure identification in situ and sometimes
by phase identification, phase composition esti- Zn-Mg and Al-Cu-Mg, Al-Fe-Si and Al-Mn-Si). eliminates the last doubts. Measurements of
mation, and phase morphology formalization. Figures 45 through 53 in the article “Selected phase microhardness values (Table 19) may also
The homogeneity and anisotropy of the structure Color Images” of this Volume show the resuts of allow some additional confirmation in attributing
parameters also should be taken into account. selective etching in various reagents. As noted a phase structure with an observed precipitate.
The description can be realized by qualitative or there, the results are not always exactly the same Quantitative Microstructure Description
quantitative analysis of images from light micro- as suggested in Table 18. Nevertheless, they (Ref 25, 27–39). Very often, the semiquantita-
scopes. The second one includes stereological should be considered as examples of the results tive description of the microstructure is adequate
analysis—estimation of the degree of the con- and as a guide for using this method in aluminum by comparative methods (according to the spe-
stituent interfaces and grain boundaries, of the alloy metallography. cial demands). Different microstructure stan-
number and size of the alloy structure constitu- Sometimes, in situ identification also is per- dards also can be used to describe the alloy
ents, and of the shape of the particles, their three- formed by x-ray microanalysis (energy-disper- microstructure. Nonetheless, standardized quan-
dimensional (3-D) morphology, size, and spatial sive spectroscopy, wavelength-dispersive spec- titative methods are demanded by customers. For
distribution. troscopy), and even x-ray diffraction phase example, standard test methods are used in de-
Fracture Analysis with the Light Micro-
scope (Ref 24, 32, 40, 41). The light micro-
scope has a limited application for observation
and identification of the fracture surface because Table 7 Applicability of the reagents for macroexaminations
of its small depth of field and resolution, in com-
parison with the electron microscope. Neverthe- Alloy Reagent Effect of etching Ref
less, the light microscope is a very useful tool Pure Al 3M Macrostructure 7–9
5M (higher HNO3 concentration
for the fracture profile observation of the metal- can improve the contrast)
lographic microsection perpendicular to the av- 6M Superficial defects
erage fracture surface. The metallographic prob- 9M Macrostructure
lem is to prepare the microsection in such a 10M, 12M
Commercial-purity Al 1M, 5M, 10M Macrostructure 7, 9
manner that the profile line will not be deformed Al-Cu 1M, 2M, 4M, 13M, 15M Reveals grain size, rolling 9
during the preparation procedure. Thus, as pre- direction, welding zone
viously mentioned, special mounting materials Al-Mn 1M, 2M, 4M, 5M, 10M, 16M Macrostructure 9
should be used for edge retention. Another rec- Al-Si 2M (cast alloys) Macrostructure 9
4M, 5M, 10M, 11M, 14M
ommended method to protect the profile line Al-Mg 1M, 2M, 4M Macrostructure 7–9
from deformation is to cover the fracture surface 8M Reveals intergranular corrosion
with a protective layer before cross-section prep- 5M, 10M, 15M and flow lines
aration (Fig. 30). Al-Mg-Si 4M Macrostructure 7–9
7M Reveals grains, depending on the
Qualitative Microstructure Description crystal orientation
and Identification of Phase Constituents. Mi- 1M, 5M, 10M, 15M Macrostructure
croscopic observation of the metallographic mi- Al-Cu-Mg-Zn 4M Macrostructure 7, 9
1M, 15M
crosection reveals the constituents of alloy mi- Al-Ti 2M Macrostructure 9
crostructure. The classical comparative method
of phase identification is by using an atlas of
micrographs from alloys of similar chemical
composition and structure. Very often, this al-
lows identification of the phase microconsti- Table 8 Typical temperature range of the heat treatment used for aluminum alloys
tuents. The first step may be the identification of Temperature range
precipitate morphology and color (Table 17) Solution annealing Aging
from a polished (unetched) microsection. Some- Alloy C F C F
times, examination of an as-polished section is Cast alloys
enough to know the alloy phase constituents.
2xx.x (Cu) 490–530 915–985 Room temp., 155–355 310–670
The next steps may involve microscopic obser- 3xx.x (Si Ⳮ Cu/Mg) 505–540 940–1005 Room temp., 155–260 310–500
vation with cross poles and etching of the mi- 4xx.x (Si) 540 1005 ... ...
crosection. If doubts remain after this second 5xx.x (Mg) 400–430 750–805 ... ...
step, the use of selective etching may be done 7xx.x (Zn) 430–590 805–1095 Room temp., 120–205 250–400
8xx.x (Sn) 480 895 220 445
for phase identification (Table 18). Selective
etching is usually complicated and time-consum- Wrought alloys
ing, but in most cases, it gives complete phase 2xxx (Cu) 495–530 925–985 160–205 320–400
3xxx (Mn) ... ... ...
identification of the material. 4xx.x (Si) ... ... ...
The selective etching procedure is very sen- 5xx.x (Mg) ... ... ...
sitive to the process conditions of time, tem- 6xx.x (Mg Ⳮ Si) 515–570 960–1060 160–205 320–400
perature, and small differences in chemical com- 7xx.x (Zn) 465–515 870–960 120 250
8xx.x (other elements) 530–540 985–1005 190 375
position of the reagents. Another very important
factor is the influence of chemical composition Source: Ref 2

termining the average grain size (e.g., ASTM E tion. From a metallographic point of view, the ● In an alloy of composition Co Cs when the
112) and the description of the dual grain size analyzed image of the microstructure should be eutectic is the nonquilibrium constituent of
(ASTM E 1181). a true representation of the material from a spec- the microstructure (Fig. 31)
Estimation of 3-D microstructural features in- imen without any defects or artifacts (scratches,
The nonequilibrium microstructure constitu-
volves analysis of images from random flats of pullouts) that can change the measurement re-
ents can result from a liquation of the alloy com-
two-dimensional (2D) section (Ref 27, 28). Pri- sults. Preparation procedures, which are in-
ponents (both additional or impurities) of high
marily, two kinds of parameters are measured: tended to enhance contrast between phase con-
partition ratio (between liquid and solid state)
stituents, are especially important in automatic
● Local (statistical) stereological parameters of and low diffusivity during solidification (Fig.
image analysis. Contrast must allow the proper
a microstructural element/particle represent 31). In the residual liquid of high concentration
establishment of the detection threshold. The dif-
an average value of a geometrical feature of of the segregated alloy components achieving
ference of gray level of the measured phase com-
the particle, such as mean volume (V), mean eutectic composition (CE), the multicomponent
ponents must be higher than the minimum de-
chord (I) of the particle, mean perimeter (L) eutectic could form at the end stage of the solid-
tection threshold. The homogeneous gray level,
of the particle, or mean surface of the particle ification process, that is, at lower temperature
that is, the quality of the microsection surface, is
section A. (TEM) than aluminum solid-solution solidified
also important from the point of view of the mea-
● Integral (global) stereological parameters rep- (To) (Table 20).
surements results. The described selective etch-
resent the digitized characteristics of structure The risk of accidental melting of the fusible
ing procedure of the phase components can im-
elements (volume, area, line length) in terms microstructure constituents (multicomponent eu-
prove the contrast between them.
of measured units, such as specific volume tectic) should be considered by a technologist for
Phase Constituent Morphology, Distribution,
fraction (Vv), specific surface of the interfaces a particular alloy or process on the basis of the
and Degree of Dispersion. The polyphase alu-
(Sv), specific length of the interfaces (PL), and industrial practice, experiments, or literature
minum alloys are characterized by the variety of
number of particles on the unit area (Na). data. The possibility of eutectic melting espe-
morphological forms—shape of precipitates,
cially should be taken into account during heat
dispersion degree, and distribution of their phase
Topological parameters are not estimated very treatment and welding, as shown schematically
or structure constituents. A uniform quantitative
often and are seldom used during standard lab- in Fig. 32. This undesirable phenomenon is a
description is difficult and must be regarded in-
oratory examinations. Quantitative description potential source of decrease in the material prop-
dividually in dependence on the examined alloy.
of microstructure more often involves measured erties and can be difficult to control or repair.
All the remarks concerning microsection quality
or calculated value of parameters concerning Eutectic Melted Zones. The following are me-
for the volume fraction measurements are valid
phase composition and the morphology, distri- tallographic problems concerning eutectic melt-
in the case of other morphological feature de-
bution or dispersion of phase constituents. Ex- ing:
scriptions. The functions of the mathematical
amples of quantitative microstructure descrip-
morphology allow the microstructure image ● Specimen preparation
tions used in estimating material properties are
modification and often can be used to improve ● Eutectic melted zone recognition on the me-
listed in Table 21.
and facilitate the establishment of the detection tallographic microsection
Phase Composition. The volume fraction of
threshold establishing (Ref 34).
phase or structure constituents is the stereologi- During cutting or mounting of the specimen
cal parameter expressing the phase composition in hot-mounting resins, preheating the specimen
of the alloy. Phase volume fraction can be esti- Specific Microstructural above TEM should be avoided. Nevertheless, be-
mated by means of the area, line, or point frac- Problems of Al-Alloy Metallography cause the solvus temperature (TS) is the limit on
tion of this phase constituent carried out on the the precipitation process in the solid state at a
flat random microsections. The automatic ana- Qualitative Description. Eutectic melted temperature lower than TEM, it is common not to
lyzer of the microscope image or the special grid zones in the microstructure of the aluminum al- exceed the solvus temperature during prepara-
on the focusing screen of the microscope can be loy may appear in the following cases: tory procedures.
used as well as the point counting in the micro- The eutectic melted zone on the metallo-
scope ocular. The measurement conditions are ● In an alloy of composition Co Cs when the graphic microsection may be visible as either
established depending on the microstructure eutectic is the equilibrium constituent of the oval or round pools filled with very dispersed
morphology and expected accuracy of estima- microstructure (Fig. 31) particles of the eutectic phases (Fig. 33, 34).
Fig. 23 Defects of the metallographic microsection preparation from cutting and mounting. (a) Overheated and deformed material during specimen cutting 400⳯. (b) Badly retained
fracture profile 500⳯

Quantitative metallography of the alumi- has more irregular (concave) features (Fig. 35). cially when porosity is in the form of many dis-
num alloys meets some specific problems con- Dispersed pores also form clusters, such as the persed clusters. Taking into account the spatial
cerning aluminum alloy microstructure regard- one shown in Fig. 35(c). At least two pores form morphology of the two kinds of porosity, one can
ing both cast and wrought alloys. a cluster. The dispersion of pores in a shrinkage- assume that the objects include isolated pores
Dispersed Porosity in Castings (Ref 34, 37). pore cluster may be different than the pore dis- and clusters from either shrinkage or gaseous po-
Dispersed porosity can be regarded as a type of persion of a gas-pore cluster. The objects visible rosity. The quantitative criterion to distinguish
microstructural constituent from the point of on the metallographic microsection are consid- the isolated and gaseous pores is their distribu-
view of image analysis and material perfor- ered similar to other microstructure constituents tion, described using the method of the nearest-
mance. In cast alloys, dispersed porosity is gen- and are measured. neighbor distance (NND) (Ref 37). Pores that
erally of two types: gas porosity and shrinkage Despite the differences in morphology, the have a distance less than an established critical
porosity. Gas porosity tends to be more convex distinction of the two kinds of porosity on the NND belong to a cluster of two pores or more;
or rounded in shape, while shrinkage porosity metallographic section can be difficult, espe- those with a greater NND are isolated.
Fig. 24 Defects of the metallographic microsection preparation from grinding and polishing. (a) Pullouts of brittle particles 250⳯. (b) Embedding of SiC abrasive particles 400⳯.
(c) Embedding of diamond abrasives 400⳯. (d) Effect of coma 250⳯. (e) Scratches from the previous step of polishing 250⳯. (f ) Scratches because of a dirty disc 250⳯

Because of the small value of the volume frac- single 3-D entity results in one 2-D image on a loys with reference to the American Foundry So-
tion of the pores (1% in good-quality alumi- random section of a metallographic flat. Volume ciety’s chart “Microstructure Control in Hypo-
num cast parts) and the large range of possible fraction of the isolated pores is then estimated. eutectic Aluminum-Silicon Alloys.”
sizes (from a few micrometers up to a few hun- The quantitative description of dispersed poros- The problem is to reveal on the metallographic
dred micrometers), the following problems ity from shrinkage should be carried out in two microsection the image of the dendrites in such
should be taken into account: steps: contrast (Fig. 36) that the automatic image ana-
lyzer may be used. Very often, the dendrites of
● The specimen surface destined for porosity ● Characteristics of shrinkage clusters (one
the ␣-aluminum solid solutions are outlined with
measurement must be well prepared to retain cluster is regarded as an individual entity) by interdendritic eutectic, but sometimes, the eutec-
pore profile and section contrast to establish the number of clusters on a measured area tic constituents have similar and too small a con-
a good detection threshold. unit trast in regard to the matrix, and their interface
● The number of measurements must be quite ● Characteristics of individual pores by means
does not form a continuous line. In this case,
large to achieve a good statistic (accuracy and of global or local stereological parameters revealing the dendritic segregation can improve
repeatability) of the results. the image quality. The mathematical morphol-
● The microscope magnification must be ad-
Dendrite Arm Size (Ref 34, 39). Dendrite arm
size (DAS) measurement is very useful, because ogy functions application for improving detec-
justed for detection of both small and large tion threshold is a method used very often in
this parameter can be considered the microstruc-
pores. quantitative metallography.
ture criterion in the Hall-Petch equation for the
The global stereological parameters of the iso- cast alloys. Dendrite arm size is also an estimator The true dendrite arm size of the n-th order
lated convex pores can be estimated by one of of the local solidification time h (Ref 34). Local measured on the metallographic microsection is:
the quantitative parameters, such as volume frac- solidification time is a very important parameter
tion (Vv), specific surface of the pore/matrix in- from the point of view of the numerical model- DASn ⳱ L/nn
terface (Sv), or number of pores per unit area on ling and simulation of the casting processes.
the metallographic microsection. These are the Daimler-Chrysler and General Motors specifi- where L is the true length of the measured line,
various methods for porosity characterization. cations for A356-T6 automotive castings include and nn is the number of arms of the n-th order
Quantitative metallography is used in the de- the method for determination of Dendritic Arm intersected by a measured line (Fig. 37a). The
scription of porosity with the assumption that a Spacing of hypoeutectic aluminum-silicon al- distance between dendrite cross-section centers
can be chosen as a measure of the DAS because
of the close correlation between these parameters
Table 9 Procedure for fine grinding (Fig. 37b). The close correlation was also stated
Step Abrasive Gradation Lubricant Rotational speed, rev/min Force for specimen, N Time, min
between DAS and a mean chord length of the
dendrite cross sections. These stereological pa-
1 SiC 500 H2O 200 50/30 1–5
2 SiC 1000 H 2O 200 40/15 1
rameters can be measured automatically by
3(a) SiC 2400 H 2O 200 40/10 2.5 means of the image analyzer (Fig. 37c).
(a) Step 3 is optional to reduce the number of subsequent polishing steps or time.
Microstructure Anisotropy. Wrought alloy mi-
crostructure is often characterized by an aniso-
tropy that results from plastic deformation. The
grains of the alloy are nonequiaxed. Special at-
tention must be given to the position of the mi-
Table 10 Procedure for mechanical polishing crosections in relation to the deformation direc-
Gradation, Rotational speed, Force for tion. The true results of the volume fraction of
Step Cloth Abrasive lm Lubricant Rev/min specimen, N Time, min the phase constituents can be estimated on the
1 Napless DP (spray or paste) 3 Alcohol based 150 40/20 1 cross sections perpendicular either to the axis of
2 With nap DP (spray or paste) 1 Alcohol based 150 40/15 1.5 rotational symmetry or to the plane of the planar
1
3a With nap DP (spray or paste) ⁄4 Alcohol based 150 40–50/10 3
3b With nap Colloidal silica suspension ... ... 150 10 0.5
symmetry (Fig. 38).
The complete microstructure description de-
Note: DP, diamond abrasive
mands two (in the case of a rotational micro-
Table 11 Reagents for electrolytic polishing and process conditions

Current
Temperature
density, Voltage, Time of
No. Electrolyte Cathode A/dcm2 V polishing Circle C F Ref
1p 820 mL H3PO4 Al 0.8–2.5 50–70 5–8 min Potentiometer 35 95 8, 23
160 g CrO3 22–30
135 mL H2SO4
100 mL distilled H2O (for all
Al alloys, except Si-Al)
2p 400 mL H3PO4 Al 35 ... 4–6 min Array 42–45 108–115 9, 23
380 mL ethanol
3p 200 mL HClO4 Stainless steel 100–400 110–220 10–25 s Array 35 95 23
800 mL ethanol 35–70
200 mL HClO4 Graphite, Al 30 50–60 2 min Potentiometer 35 95
1000 mL ethanol 20
4p 50 mL HClO4 Al, stainless steel 50–55 10–15 10–25 s Array 35 95 8, 9, 23
1000 mL CH3COOH 25–30
(glacial)
5p 62 mL HClO4 (70%) ... 3.85 A/cm2 ... 20 s ... Rinse in warm water, 7
700 mL ethanol prevent overheating,
10 mL 2-butoxyethanol use 10 s steps, cool
137 mL distilled H2O specimen

structure symmetry) or even three (in the case of tion by means of its qualitative or quantitative In most cases, the qualitative results (EDS
a planar microstructure symmetry) oriented mi- chemical composition estimation in the mic- spectrum with identified peaks of a characteristic
crosections to be prepared and analyzed. The roregions (Fig. 41) line) show the local chemical composition of
precautions that were mentioned in the section
“Specimen Cutting” in this article must be re-
spected. In the recrystallized alloys, the grains
may have asymmetric or even bimodal grain size
distributions, so the microscope magnification
must be chosen in such a manner that both large
and small grains may be revealed, detected, and
measured. The shape of the grain size distribu-
tion is influenced by the measure conditions; for
example, the length of the measure line.
SEM Examination
X-Ray Microanalysis (Ref 42). As noted, x-
ray microanalysis of the chemical composition
with modern SEM systems is a very useful tech-
nique in microstructural analysis of selected
microregions of the specimen. Most SEMs in
modern metallographic laboratories are
equipped with x-ray analyzers of either the en-
ergy-dispersion spectrum (EDS) or, less widely,
the wavelength-dispersion spectrum (WDS).
Due to the strictly localized interference of the
electron beam and specimen material, the iden-
tification of the chosen particular phase precipi-
tates may be carried out. This facility is of great
importance in the case of multiphase aluminum-
alloys, when the phase constituent precipitates
very often have similar morphology and color
during observation under the metallographic
light microscope. In this situation, x-ray micro-
analysis is an easy and repeatable method to un-
equivocally verify the phase composition of the
alloy. The EDS mode of x-ray microanalysis Fig. 25 Lightening effects to enhance contrast between phase constituents in an unetched specimen of Al-Si-Cu-Ni
gives fast measurements of the local chemical alloy. (a) Bright-field illumination with silicon (A, dark gray), ␣-Al(FeMn)Si (B, light gray), and Al2Cu (C, beige).
composition results, comparable with WDS (b) Dark-field illumination with phase boundaries revealed. (c) Cross-poles mode of observation with silicon (dark violet),
␣-Al(FeMn)Si (light violet), and Al2Cu (light pink). (d) Phase contrast: silicon (dark violet), ␣-Al(FeMn)Si (dark pink), and
from the point of view of accuracy and detection Al2Cu (pink-yellow with blue contrast on the interfaces). All at 1000⳯. For color version, see Fig. 41 of the article “Selected
limit for elements of Z 11. Color Images” in this Volume.
The complementary use of classical metallog-
raphy and x-ray microanalysis helps resolve the
following problems (Fig. 39–41). Table 13 Reagents for chemical polishing
● Phase identification in a multiphase alloy Temperature
(Fig. 39) or verification of the selective etch- No. Chemical composition Time of polishing C F Remarks, Ref
1
ing results 1ch 80 mL H3PO4 ⁄4–5 min, depending on flatness 80 175 Al and Al
35 mL HNO3 of surface alloys, 23
● Verification of structure observations using
cross poles (Fig. 40) 2ch 700 mL H3PO4 2–6 min 100–120 210–250 Al alloys, 23
● Key for phase designation: phase identifica- 30 mL HNO3
120 mL CH3COOH (glacial)
3ch 100–170 mL HNO3 15–30 s 50–80 120–175 Pure Al, 9, 23
100–200 g NH4HF
Table 12 Electrochemical potential of 0.08–0.8 g PbSO4
aluminum and some intermetallic phases in 1000 mL distilled H2O
10–20 mL HNO3 5–30 s 50–60 120–140
3% NaCl
10–20 mL saturated water
Phase Potential, mV solution of NH4HF
0.08–0.8 g PbSO4
Al4N ⳮ750
65–80 mL distilled H2O
Mg2Si ⳮ1250
4ch 1 p. HNO3 10–30 min 0 32 Al alloys, 7
Al3Mg2 ⳮ930
1 p. ethanol After finish, mechanical grinding
MgZn2 ⳮ790
1% or less H2O2 (optimum on paper of gradation 600
Al6Mn ⳮ607
depends on alloy polished) Mechanical stirring
Al2Cu ⳮ370
5ch 25 mL H2SO4 30 s–2 min 85 185 Al alloys, 9
Al3Ni ⳮ210
70 mL H3PO4
Al3Fe ⳮ140
5 mL HNO3
Source: Ref 25 160 mL distilled H2O

chosen particles or microregions and are suffi- images. The SEM makes it possible to reveal the necessary, but removing the superficial deformed
cient to solve these problems. 3-D morphology of polyphase regions as inter- or contaminated layer can shorten the process.
One of the demands of x-ray spectrum acqui- dendritic eutectic or intermetallic phase precip- Scanning electron examination of deep-
sition is a flat and clean sample surface. In the itates. The specimen preparation procedure con- etched specimens is a method often used in the
case of aluminum alloys, it is rather difficult be- sists of dissolving the aluminum matrix in a analysis of modification effects on aluminum-
cause of their strong tendency for oxidation. To reagent that will not attack the eutectic compo- silicon eutectic or primary silicon precipitates in
improve the contrast of the matrix/phase inter- nents or intermetallic phase precipitates. The re- aluminum-silicon cast alloys. The process of
face, slight etching is acceptable. siduals of the etching products should be re- nucleation of the secondary phases on the ma-
SEM Observation of Deep-Etched Micro- moved by intensive rinsing in tap water (in the trix/primary phase interfaces also may be in-
sections (Ref 2, 43). The polyphase structure case of alcohol-based reagents, alcohol for rins- vestigated with this method (Fig. 42, 43).
formed during alloy solidification is character- ing is recommended). Short rinsing in the ultra- SEM Observation of the Fracture Surface
ized by 3-D morphology, which is often difficult sonic cleaner gives very good results. The pre- (Ref 24, 32, 44). Topography of fracture sur-
to reconstruct on the basis of 2-D cross-section liminary preparation of the specimen is not faces is commonly examined by SEM. The large
depth of field is a very important advantage for
fractographic investigations (Fig. 44). Fracture
surfaces can be observed by means of SEM with-
out almost any special preparation; nevertheless,
if it is possible, the specimens should be exam-
ined immediately after failure because of the
very fast superificial oxidation of aluminum and
its alloys. In some cases, for example, after a
catastrophic crack, the specimen should be
cleaned mechanically by rinsing in ultrasonic
cleaner, chemical reagents, or electrolytes.
Analysis of the SEM fracture images helps in
the identification of:
● The specific failure mechanism
● The fracture path in structure constituents
● The microregion of crack initiation
● The areas of local inhomogeneous strain state
● The morphological features of the observed
fracture area
Fig. 26 Lightening effects to reveal contrast of crystal orientation in an etched aluminum-copper specimen. (a) Bright-
field illumination with ␣-Al (light gray) and Al2Cu (gray). (b) Dark-field with phase boundaries revealed. (c) Fig. 27 Effect of etching in revealing grain boundaries
Cross-pole mode of observation revealing Al2Cu crystal orientation in color image. (d) Phase contrast in color image. All of solution annealed (552 C, or 1025 F, for 1
etched with 0.5% HF. Magnification 200⳯. For color version, see Fig. 42 of the article “Selected Color Images” in this h, water quenched) Al-4%Cu alloy. Keller’s reagent (7m in
Volume. Table 4). 200⳯
Table 14 Reagents for electrolytic microetching

Current density,
No. Electrolyte Cathode A/dcm2 Voltage, V Time of etching Remarks, Ref
1me 4–5 mL HBF4 Al, stainless steel, Anodize: 0.2 A/cm2 20 V/dc 40–80 s Check results on microscope with
200 mL H2O lead Etch: 20–40 V/dc Al-4N: 1–2 min cross poles; reveals grain
(Barker’s reagent) Al-Mn1: 1–1.5 min structure or general structure in
Al-Mg-Si0.5: 1.5–2.0 min most series of wrought alloys
Al-Cu-Zn-Mg: 2–2.5 min 7, 9, 10
Al-Mg: 2.5–3.0 min
Al-Mg-Si: 3–3.5 min
2me 10 mL H3PO4 Stainless steel ... 1–8 V/dc 5–10 s Reveals grain structure or general
90 mL distilled H2O structure in most series of
wrought alloys
7, 9, 10

Examples are shown in Fig. 44 and 45. Figure ticles of the intermetallic phase g(MgZn2). The g(MgZn2). The very elongated, large hollows
44 is an example of a transgranular ductile frac- dimpled microvoids in the deformed material were produced by a coalescence of the arrays of
ture. The crack developed through aluminum arose round these particles, and the first stage of smaller voids, and they were separated with the
solid solution hardened with the dispersed par- the decohesion took place on the ␣-aluminum/ long tear ridges on the top of the shear micro-
Table 15 Applicability of the reagents for chemical microetching, commonly recommended

Grain boundaries, interfaces,
size and shape of Microsegregation of Phase constituent Deformation Recrystallization Heat treatment
Alloy group phase constituents alloy components identification effects effects effects
1xxx (wrought) 5m, 7mB ... ... ... ... ...
2xxx (wrought) 4m, 5m, 7mA, B, 22m, 24m 7mA, B, 22m 1m, 2m, 10m 7m, 22m 7m, 22m, 24m 1m
3xxx (wrought) 5m, 7mB 14m 1m, 2m, 10m ... ... ...
4xxx (wrought) 5m, 7mA, B ... ... ... ... ...
5xxx (wrought) 1m, 4m, 5m, 7mA, B, 9m, 10m 14m ... 10mB 3% Mg ... ...
6xxx (wrought) 1m, 4m, 5m, 7mB, 10m ... 1m, 2m, 4m, 5m, 10m ... 19m, 24m 7m, 22m
7xxx (wrought) 4m, 5m, 7m ... 1m, 2m, 5m, 7mA, 20m 7m, 22m 10mB, 23m, 24m 7mB
Cast alloys 7mA, B, 9m, 15mB, 11m, 12m, 13m, 14m (Al-Mg) 1m (Al-Cu), 2m, 3m, 4m, 5m, 6m, 7mA ... ... ...
22m, 24m (Al-Si), 9m, 10mB (Al-Cu, Al-Mg, Al-
Mg-Si), 15m, 16m, 17m, 18m, 19m,
20m
Source: Ref 5, 7–17, 23, 26
Fig. 28 Effect of etching in revealing phase boundaries of an Al-Si-Zn-Cu alloy at 500⳯. (a) Unetched. (b) Etched with 5m Ⳮ 15m (solution B) reagents (Table 4)
Fig. 29 Effect of etching in revealing phase constituents of alloy 390 etched with reagent 5m (Table 4). (a) Etched for 1 s. (b) Etched for 10 s. Both at 500⳯

regions. On the walls of the tear ridges, the oval face of an as-cast state 356 alloy tensile-test itates of the eutectic silicon. The area of the
shear dimples are visible (Fig. 44b). Such frac- specimen is shown in Fig. 45. The morphology crack initiation is visible in the center of Fig.
ture morphology testifies to the inhomogeneous from transgranular brittle fracture (cleavage) is 45(a). The fracture then went through the
stress state. mainly visible, but some degree of plastic de- cleavage planes in the silicon particles. In the
An example of a mixed-mode fracture sur- formation in the aluminum solid solution also bottom part of Fig. 45(b), the dendrites of alu-
face (with indications of brittle and ductile may be noticed in the form of shallow dimples. minum solid solution were visible in the
cracking on a microscopic scale) from the sur- The first decohesion took place in the precip- shrinkage microarea.
Table 16 Microscopic techniques for metallographic examination of the alloy

microstructure
Microscopic technique
Transmission electron
Structure type, concentration Light microscope microscope Scanning electron microscope
range of alloying element Resolution: 300 nm Resolution: 2–3 nm Resolution: 4–9 nm
Pure solid solution Grain size Dislocation structure Fracture morphology
(commercial-purity Al) Anisotropy Stacking faults Material defects
Material defects
Inclusions
Dispersed precipitates with Grain size Dislocation structure Fracture morphology
alloy concentration less Anisotropy Disperse precipitates Material defects
than the maximum limit of Material defects—chemical or morphology and Disperse precipitates
solid solubility structural heterogeneity distribution morphology and
Inclusions PFZ distribution of PFZ on
Disperse particles distribution Stacking faults fracture surface or deep-
PFZ etched section
Eutectic or peritectic Grain size Dislocation structure Fracture morphology
solidification with alloy Structure anisotropy Disperse precipitates Material defects
concentration greater than Dendrite morphology morphology and Phase precipitates
the maximum limit of Structure defects distribution morphology and
solid solubility Chemical or structural PFZ distribution on deep-etched
heterogeneity Interface morphology section
Inclusions Stacking faults
Phase precipitates morphology
and distribution
PFZ
Note: PFZ, precipitate-free zones
Fig. 30 Fracture profile from etched transverse microsection of two aluminum-silicon alloys. (a) Alloy 356.0 alloy at a magnification of 50⳯. (b) Alloy 390.0 at a magnification of
500⳯. Both etched with reagent 5m (Table 4)

Table 17 Example of the most common phase constituents identification procedure in commercial aluminum alloys
Color of precipitates Identification
Morphology Phase under light microscope Birefringes Other methods(a)
Needles b-AlFeSi Gray Moderate, light to dark gray Selective etching, EDS
Al7Cu2Fe Light gray, outlined Moderate, light to dark gray Selective etching, EDS
Al3Fe Gray ... Selective etching, EDS
Polyhedra Si Blue-gray None Selective etching, EDS
Al6Mn, Al6(FeMn) Gray Strong, light to dark gray Selective etching, EDS
Primary Al6CuMg4 Light yellow, white ... Selective etching, EDS, BSED
Primary ␣-Al(TM)Si(b) Light gray ... Selective etching, EDS, BSED
Chinese script Si Blue-gray None Selective etching, EDS
Mg2Si Blue None Selective etching, EDS
␣-AlMnSi Gray ... Selective etching, EDS, BSED
AlCuFeMn Light gray ... Selective etching, EDS, BSED
␣-AlFeSi Light gray None Selective etching, EDS, BSED
␣-Al(TM)Si(b) Gray-brown, depending on Mn, Cr contents None Selective etching, EDS, BSED
Al8FeMg3Si6 Light gray, not outlined Strong, from yellow to blue Selective etching, EDS
Al3Ni Light gray, outlined ... Selective etching, EDS, BSED
Al7Cu4Ni Light gray ... Selective etching, EDS, BSED
Plates, irregular Si Blue-gray None Selective etching, EDS
Al9FeNi Gray, outlined ... Selective etching, EDS, BSED
Al4FeSi2 Gray, outlined ... Selective etching, EDS, BSED
Al3FeSi Gray ... Selective etching, EDS, BSED
Rounded, irregular Al2Cu Pink-yellow, outlined Strong, orange-greenish-blue Selective etching, EDS
particles Al2CuMg Darker than Al2Cu Very strong, yellowish-red, green-blue Selective etching, EDS, BSED
Al3Mg2 White, brighter than matrix None Selective etching, EDS
AlCuMg-MgZn2 Light, slightly outlined Slight change from light to dark gray Selective etching, EDS, BSED
Al6CuMg4-Al2Mg3Zn3 Light yellow, white None Selective etching, EDS, BSED
Al5Cu6Mg2-Mg2Zn11 Light, slightly outlined ... ...
Al5Cu2Mg8Si6 Bright yellow, outlined Strong, from orange to blue Selective etching, EDS, BSED
Rosettes Al3Fe Gray Slightly visible EDS
(a) EDS, energy-dispersive spectroscopy; BSED, backscattered electron diffraction. (b) TM, transition metal. Source: Ref 5, 7–17, 26

Table 18 Phase identification by selective microetching procedure

Reagent (Table 4) and effects
Phase 1m 2m 3m 4m 5m 6m 9m 13m 15m 17m 18m 19m 27m
Si ... Not attacked ... ... Outlined ... Outlined ... Dark blue, Dark blue, ... ... ...
(Ref 8) (Ref 5) (Ref 5) brown 30 s; violet,
(Ref 14) 150 s
(Ref 16)
␣-Al ... ... ... ... Grain ... Grain Micro- Grain ... ... ... ...
boundaries boundaries segre- boundaries
(Ref 8) (Ref 8) gation (Ref 14)
(Ref 14)
Al9Co2 Not attacked Etched Dark (Ref 8) Dark (Ref 8) Brown Brown ... ... ... ... ... ... ...
(Ref 8) (Ref 8) (Ref 8) (Ref 8)
Al2Cu Red (Ref 8, Not attacked Dark (Ref 8) Dark (Ref 8, Pink Not attacked ... ... ... Yellow, 30 s Slightly Blue ...
26) (Ref 8) 26) (Ref 26) (Ref 8) Green 150 s tinted (Ref 17)
Dark (Ref 2) Brown (Ref Not attacked (Ref 16) (Ref 11, 12)
11) (Ref 8)
Al7(CrFe) Not attacked Not attacked Blue (Ref 8) Blue (Ref 8) Pale brown Not attacked Outlined ... ... ... ... ... ...
(Ref 8) (Ref 8) (Ref 5) (Ref 8) (Ref 5)
Al3Fe ... Black Dark (Ref 8) Dark (Ref 8, Etched ... Dark brown/ ... ... ... ... ... ...
(Ref 5) 26) (Ref 17) dark blue
Etched Not etched (Ref 2)
(Ref 4) (Ref 7)
Al3Mg2 Etched Etched Not attacked Not attacked Outlined Slightly Outlined ... ... ... ... ... Brown
(Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 17) etched (Ref 5) (Ref 17)
Light blue (Ref 8)
(Ref 5)
Slightly
etched
(Ref 8)
Al6Mn Not attacked Not attacked Bright blue Brown Slightly Not attacked Not attacked ... ... ... ... ... ...
(Ref 8) (Ref 7) (Ref 8) (Ref 8) etched (Ref 8) (Ref 5)
(Ref 8)
Al6(MnFe) ... Not attacked Slightly Dark (Ref 8) Dark gray Black Etched ... ... ... ... ... ...
(Ref 8) etched (Ref 17) (Ref 8) (Ref 2)
(Ref 8) Unetched
(Ref 4)
Al3Ni Not attacked Slightly Bright brown Dark (Ref 8), Dark (Ref 8) Brown Not outlined, ... ... ... Brown ... ...
(Ref 8) etched (Ref 8) outlined (Ref 11) darkened (Ref 11, 12)
(Ref 8) brown- (Ref 5)
blue
(Ref 5)
Al3Ti Not attacked Not attacked Not attacked Dark (Ref 8) Outlined, Not attacked Light gray ... ... ... ... ... ...
(Ref 8) (Ref 8) (Ref 8) darkened (Ref 8) (Ref 5)
(Ref 5)
CaSi2 ... ... ... ... Dark blue ... Outlined, ... ... ... ... ... ...
(Ref 13) darkened
(Ref 5)
Mg2Si Attacked Etched Not attacked Brown Blue (Ref 5, Darkened Blue-brown ... ... ... ... ... ...
dissoluted (Ref 7) (Ref 8) (Ref 11) 26) (Ref 11) (Ref 5)
(Ref 26) Darkened Unetched
(Ref 11) (Ref 8)
MgZn2- Etched Etched Not attacked Not attacked Outlined Brown Outlined, ... ... ... ... ... ...
AlCuMg (Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 13, (Ref 8) black
17) (Ref 5)
Brown
(Ref 5)
Al18Cr2Mg3 Etched Etched Not attacked Not attacked Not attacked Not attacked Outlined ... ... ... ... ... ...
(Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 5)
Al7Cu2Fe Darkened Black Dark (Ref 8) Dark (Ref 8) Outlined Dark (Ref 8) Not attacked ... ... ... ... ... ...
(Ref 8) (Ref 8) (Ref 5) (Ref 5)
Not attacked
(Ref 8)
Al6CuMg4- Dark, red- Black Dark (Ref 8) Dark (Ref 8) Black Etched ... ... ... ... ... ... ...
Al2Mg3Zn3 brown (Ref 13) (Ref 8)
(Ref 8) Etched
(Ref 8)
A2CuMg Outlined Not attacked Not attacked ... Unetched, Dark Dark (Ref 5) ... ... ... ... ... ...
(Ref 5) (Ref 8) (Ref 8) gray (Ref 2, 8)
Dark (Ref 4) (Ref 13)
Black
(Ref 5)
Al20Cu2Mn3 Not attacked Not attacked Not attacked Not attacked Brown-blue Not attacked Dark brown ... ... ... Blue ... ...
(Ref 8) (Ref 8) (Ref 8) (Ref 8) (Ref 5) (Ref 8) (Ref 5) (Ref 11)
Not attacked
(Ref 8)
Al7Cu4Ni ... ... Not attacked ... Darkened ... Not attacked ... ... ... ... ... ...
(Ref 8) (Ref 5) (Ref 5)
Al9FeNi Not attacked Not attacked Dark (Ref 8) Dark (Ref 8) Outlined Brown Outlined, ... ... ... Dark ... ...
(Ref 8) (Ref 8) (Ref 5, 17) (Ref 8) darkened (Ref 11, 12)
Dark brown Blue-violet (Ref 5)
(Ref 8) (Ref 11)
(continued)

Table 18 (continued)
b-AlFeSi Slightly Etched (Ref ... Etched (Ref Light brown ... ... ... ... ... Brown-blue ... ...
etched 8, 26) 8, 26) (Ref 26) (Ref 11, 12)
(Ref 26) Dark (Ref 8)
Unetched Darkened
(Ref 8) (Ref 7)
␣-AlFeSi Slightly Slightly Not attacked Not attacked Outlined Not attacked Outlined, ... ... ... ... ... ...
etched etched (Ref 8) (Ref 8) (Ref 5) (Ref 8) darkened
(Ref 8) (Ref 8) Not attacked (Ref 5)
(Ref 8)
␣-AlMnSi Not attacked Not attacked Not attacked Pale brown Outlined Not attacked Outlined ... ... ... ... ... ...
Not attacked
(Ref 8)
␣-AlFeMnSi Slightly Etched (Ref ... ... Light brown ... Brown/1 min ... Gray ... ... ... ...
etched 7, 8, 26) (Ref 26) (Ref 5) (Ref 14)
(Ref 8, Unetched
26) (Ref 8)
Al18Mg3Mn2 ... ... ... Not attacked Outlined ... Outlined ... ... ... ... ... ...
(Ref 8) (Ref 5) (Ref 5)
Al5Cu2Mg8Si6 Blue Dark ... Dark Brown-black ... Not attacked ... ... ... ... ... ...
Al8Mg3FeSi2 Brown Etched ... Slightly Bright gray, ... Slightly ... ... ... ... ... ...
(Ref 26) (Ref 26) etched outlined etched
(Ref 26) (Ref 26) (Ref 26)
Not attacked
(Ref 5)
Table 19 Hardness of chosen intermetallic Table 20 Temperature of the eutectic transformation in multicomponent aluminum alloys
phases in aluminum alloys Temperature
Phase Microhardness, HV (MN/m2) No. System C F Eutectic phases
Al 1200–1400 1 Al-Cu 548 1018 ␣-Al Ⳮ Al2Cu
Al2Cu 4000–6000 2 Al-Mg 450 840 ␣-Al Ⳮ Al3Mg2
Al9Co2 6500–7500 3 Al-Li 180 355 ␣-Al Ⳮ Al4Li9
Al8Mg5 2000–3400 4 Al-Si 577 1006 ␣-Al Ⳮ Si
Al2CuLi 4250–5200 5 Al-Sn 231 448 ␣-Al Ⳮ Sn
Al6Cu3Ni 10,000 6 Al-Zn 277 531 ␣-Al Ⳮ Zn(Al)
Mg2Si 4500 7 Al-Cu-Mg 449 840 ␣-Al Ⳮ Al6CuMg4 Ⳮ Al8Mg5
Al3Fe 9600–11,500 8 Al-Cu-Si 495 925 ␣-Al Ⳮ Al2Cu Ⳮ Si
b-AlFeSi 5800 9 Al-Cu-Fe 545 1015 ␣-Al Ⳮ Al2Cu Ⳮ Al7Cu2Fe
␣-AlFeSi 9580 10 Al-Fe-Si 576 1069 ␣-Al Ⳮ Al5FeSi Ⳮ Si
Al6FeMn 7040 11 Al-Mg-Si 448 838 ␣-Al Ⳮ Mg2Si Ⳮ Al8Mg5
␣-AlFeMnSi 8000–9000 12 Al-Mg-Zn 447 837 ␣-Al Ⳮ Al2Mg3Zn3 Ⳮ Al8Mg5
MgZn2 2500 13 Al-Mn-Si 547 1017 ␣-Al Ⳮ ␣-AlMnSi Ⳮ Si
Si 8700–13,500 14 Al-Cu-Mg-Si 444 831 ␣-Al Ⳮ Al6CuMg4 Ⳮ Al8Mg5 Ⳮ Mg2Si
Al6Mn 5400–5600
Al9FeNi 6900–7400
Al3Ni 7000–7700
Al7Cr 5000–7000
Al3Ti 4000–7000 Aluminum Casting Alloys, Edimet, Brescia, Prakt. Metallogr., Vol 21 (No. 5), 1984, p
Al3Zr 4270–7400 1993 258–268
Al20Cu2Mn 4200 6. Struers—The Best of Structure 1–12, Co- 14. E. Weck and E. Leistner, Metallographic In-
Al8FeMg3Si6 2700
Al5Cu2Mg8Si6 4500 penhagen, 1988, p 101–104 structions for Colour Etching by Immersion,
Al18Cr2Mg3 4600–5000 7. Metallography and Microstructures, Vol 9, Part III, Deutscher Verlag fur Schweisstech-
Source: Ref 3 Metals Handbook, 9th ed., American Soci- nik-GmbH, Dusseldorf, 1986
ety for Metals, 1985, p 351–388 15. M. Richard, Reactif Micrographic pour Col-
8. M. Orman, Metalografia Aluminium (Met- orer le Silicium Dans les Alliages d’Al (Me-
allography of Aluminum), Wyd. Śla˛sk, Ka- tallographic Reagent for Coloration of the
REFERENCES towice, 1957 Silicon Precipitates in Aluminum Alloys),
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Alloys, ASM Specialty Handbook, ASM In- 11. E. Beraha and B. Shpigler, Color Metallog- of structure 1–12, Copenhagen, 1988, p
ternational, 1993 raphy, American Society for Metals, 1977 101–104
3. L.F. Mondolfo, Aluminum Alloys: Structure 12. E. Beraha, Metallographic Reagents Based 17. G. Vander Voort, Ed., Applied Metallogra-
and Properties, Butterworths, 1976 on Molybdate Solutions, Prakt. Metallogr., phy, Van Vostrand R., 1986
4. J.E. Hatch, Aluminum—Properties and Vol 11 (No. 5), 1974, p 271–275 18. U.R. Kattner, Al-Fe (Aluminum-Iron), Bi-
Physical Metallurgy, American Society for 13. R. Poganitsch, R. Sigl, and F. Jeglitsch, Se- nary Alloy Phase Diagrams, 2nd ed., T.B.
Metals, 1984, p 30–31 quential Etching for the Identification of Massalski, Ed., ASM International, 1990, p
5. E. di Russo, The Atlas of Microstructures of Phases in Technical AlZnMgCu Alloys, 149

Table 21 Some examples of quantitative descriptions of microstructure for material properties examination
Microstructure factor Microstructure feature Method of estimation(a) Structure criterion(b) Ref
Phase composition Vv (phase volume fraction) for solid Measured directly r ⳱ r␣Vv␣ Ⳮ rbVvb 29
solution (V␣v ) or separate phases (Vvsp) Pz (Zener drag) ⳱ 3cVv/d 40, 41
Dispersion factors d (grain diameter) Measured directly or calculated by using Re ⳱ kdⳮ1/2 31
DAS (dendrite arm size) measured parameters: UTS ⳱ k Ⳮ k1dⳮ1/2 Ⳮ k2DASⳮ1/2 32, 33
d (interlamellar space in eutectic) DAS ⳱ 1/Nl R0.2 ⳱ k Ⳮ k3dⳮ1/2 Ⳮ k4DASⳮ1/2 32, 33
r (precipitates radius) I ⳱ Vv/Nl DAS ⳱ Khn 34, 41
I ⳱ mean intercept length r ⳱ X{P(r rc)Vv1/2 Ⳮ P(r rc)1.5 V1/2
v /r} 35
Nl ⳱ linear number density
Shape factors e (particle elongation) Calculated by using measured parameters Kn ⳱ Fa/Fb 31, 36
(e.g., Feret diameter, F): Kn ⳱ stress concentration factor
e ⳱ Fa/Fb
Fa ⳱ maximum (Feret) diam.
Fb ⳱ diam. orthogonal to Fa
DE (equivalent round particle diameter) Calculated by using measured parameters: VGP ⳱ rc/DE 30
DE ⳱ (4A/p)1/2, with A ⳱ mean
surface of particle section
DE ⳱ 2(Vv/pNa)1/2, with Na ⳱ number
of particles on unit area
Roundness (C) CL ⳱ pPL/2AA
PL ⳱ number of intersections of surfaces
with unit test line
AA ⳱ area fraction
Distribution l ⳱ mean particle spacing Calculated by using measured parameters: s ⳱ G•b/l 31
l ⳱ 1/Nl
k ⳱ mean free path Calculated by using measured parameters: 36
k ⳱ (1 ⳮ Vv)/Nl
(a) Source: Ref 13, 15, 27, 30, 32, 36, 37. (b) r, stress; c, grain boundary energy; Pz, Zener drag; c, strengthening of solid solution; Re, yield stress; UTS, ultimate tensile strength; R0.2, yield strength; h, local solidification
time; X, strengthening constant; Kn, stress concentration factor; VGP, void growth propagation rate; s, shear stress; G, shear modulus; b, Burgers vector. k, k1, k2, k3, k4, and K are empirical coefficients, r␣ and rb stress in ␣
phase and b phase, respectively.
Table 22 Reagents used for deep etching of aluminum alloys

No. Chemical composition Etching mode Purpose or application Ref
1s A) 10 mL HCl 24 h in reagent A, then 1 h in reagent B Dissolves Al matrix and reveals Si 17
90 mL distilled H2O
B) 2.5 mL HCl
2 mL HNO3
0.75 mL HF
40 mL distilled H2O
2s A) 15 mL HCl 30–60 min with A, then 2–4 min with B, Dissolves Al matrix; reveals eutectic Si 42
10 mL HF 15–30 C (60–85 F), 20 min morphology
90 mL distilled H2O
B) 25 mL HNO3
90 mL distilled H2O
3s 10 mL HCl Approximately 60 min Dissolves Al matrix; reveals Si 17
90 mL distilled H2O morphology
25 mL HCl 15–30 min
75 mL distilled H2O
4s 2 g K1 1) Electrolytic etch at 2–5 V, 5–20 min., Dissolves Al 17
wash in methanol
2) Raise in 30 s voltage 0–30 V, 30 s,
stirring, 0.3 A/mm2, clean
ultrasonically in methanol for 30 s
5s 0.25–0.5 N solution of HgCl2 in distilled 5–15 min Dissolves Al matrix; reveals details of Si 42
water crystal morphology
6s 30% solution of NaOH in distilled water 3–20 min, 70 C Dissolves Al matrix; reveals details of Si 42
eutectic, intermetallic phase
morphology
7s 3 g NaOH 3 min–2 h Dissolves Al matrix; reveals details of Si 42
3 g Na2CO3 eutectic, intermetallic phase
8s 10 mL H3PO4 13 min–1 h, 50 C (120 F) Dissolves Al matrix; reveals primary Si 42

Fig. 31 Schematic of microstructure constituents formed with alloying variations in eutectic melting zones. Co, average
alloy composition; CE, eutectic composition achieved by liquation into residual liquid during nonequilibrium
solidification; Cs, limit of solid solubility in the aluminum-solid solution; To, solidus temperature for average alloy com-
position; TEM, local solidus temperature for eutectic composition, or temperature of eutectic melting; TS, solvus temperature
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438 1998, p 445–449 39. M. Warmuzek, Dendritic Microstructures in
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Fig. 32 Schematic of eutectic melting regions during (a) heat treatment and (b) welding. TH, temperature of annealing;
TEM, temperature of eutectic melting; To, alloy solidus temperature. Dark areas represent regions of eutectic
melting.
Fig. 33 Round islands of nonequilibrium eutectic in micrograph of 355 alloy at (a) 700⳯ and (b) 1500⳯

Fig. 34 Examples of eutectic melting microstructures (a) Alloy 2014-T6 closed-die forging, showing rosettes formed by eutectic melting when the solidus temperature (510 C, or
950 F) was exceeded during solution heat treating. Other constituents are particles of CuAl2 (white, outlined) and insoluble (Fe, Mn)3SiAl12 (dark). Keller’s reagent. 500⳯
(b) A354-T4 investment casting with fusion voids (black) caused by eutectic melting when solidus was exceeded in solution heat treatment. Surface of casting is blistered. Gray particles
are eutectic silicon. 0.1% HF. 50⳯ (c) As-cast alloy D712-F with intergranular fusion voids (black) caused by eutectic melting as a result of exceeding the solidus temperature during
dip brazing, Keller’s reagent. 100⳯
Fig. 35 Micrographs of porosity in a cast aluminum-silicon alloy. (a) Gaseous porosity. 100⳯. (b) Dispersed shrinkage porosity. 50⳯. (c) Cluster of shrinkage pores. 50⳯. Source:
Ref 38

Fig. 36 Image contrast (left) and corresponding black-and-white (b-w) detection thresholds (right) for automatic image
analysis of dendrite arm size in hypoeutectic aluminum-silicon cast alloys. (a) Good contrast for automatic Fig. 37 Measure methods of dendrite arm size (DAS).
image analysis of dendrite outlined with ␣-Al Ⳮ Si eutectic. 200⳯. (b) Poor contrast for automatic image analysis of (a) True DAS (k). (b) Mean distance between
dendrite outlined with ␣-Al Ⳮ Si eutectic. 100⳯. (c) Dendrite revealed by color etching (shown here in black and white) dendrite cross-section centers (Lp). (c) Mean chord length
with Weck I reagent (13m in Table 4) with detection in black-and-white mode. 800⳯ of dendrite cross sections (Lc). Source: Ref 34, 39

Fig. 38 Microstructure anisotropy. (a) Schematic views of microstructural anisotropy in cylindrical and rectangular
sections. (b) Transverse (left) and longitudinal (right) view of anisotropy in solidification microstructure from
directional cooling of aluminum-copper eutectic alloy. 400⳯. (c) Transverse (left) and longitudinal (right) view of aniso-
tropy from plastic deformation of hot-rolled 3004 alloy. 500⳯. Etched with 0.5% HF (5m in Table 4)

Fig. 39 Example of energy-dispersion spectrum (EDS)-aided metallography for phase identification of (a) a silicon
primary precipitate in an unetched specimen of aluminum-silicon cast alloy at 1000⳯, and (b) an AlFeSi
primary precipitate in an etched (0.5% HF) specimen of AlSiFe cast alloy at 500⳯

Fig. 40 Example of energy-dispersion spectrum (EDS)-aided metallography in interpretation of color images in polar-
ized light. The P phase (Al8FeMg3Si6) in an AlSiCuNi alloy is indicated by EDS for micrographs with (a) first
position of cross poles and (b) second position of cross poles. Etch, 0.5% HF. 500⳯. For color version, see Fig. 43 of the
article “Selected Color Images” in this Volume.

Fig. 41 Example of energy-dispersion spectrum (EDS)-aided metallography as a key for phase identification in an Al-
Si-Cu-Ni alloy. (a) Image of etched specimen (0.5% HF) at 500⳯. (b) EDS of Mg2Si (A, blue precipitate). (c)
EDS of Al3NiCu (B, light-brown precipitate). (d) EDS of Al8Fe(Ni)Mg3Si6 (C, gray precipitate). (e) EDS of ␣-aluminum matrix
(light-background). (f ) EDS of eutectic silicon (D, dark gray precipitate). For a color version of micrograph, see Fig. 44 of
the article “Selected Color Images” in this Volume.

Fig. 42 Modified and unmodified phase morphology of a eutectic aluminum-silicon alloy from examination by light microscopy (left, at 750⳯) of etched specimens (0.5% HF)
and by SEM imaging (right, at 4000⳯) of specimens deep etched with procedure 2s in Table 22 [Solution A (Flick’s reagent) Ⳮ Solution B]. (a) Unmodified alloy. (b) Modified
alloy

Fig. 43 Morphology of intermetallic phases examined by light microscopy (left) of etched specimens (0.5% HF) and by SEM imaging (right) of specimens deep etched with Flick’s
reagent. (a) b-AlFeSi phase particles in the interdendritic region of an unmodified hypoeutectic aluminum-silicon alloy. (b) Chinese script particles of ␣-AlFeSi phase in the
interdendritic region of a modified hypoeutectic aluminum-silicon alloy. (c) Al6FeMn phase particles in the interdendritic region of alloy 3004

Fig. 44 SEM images, at two magnifications, of transgranular ductile (microvoid coalescence) fracture surface in hot-
rolled 7050 alloy after T6 heat treatment. At the higher magnification (b), the oval shear dimples on the tear
ridges indicate an inhomogeneous stress state.
Fig. 45 SEM images of a mixed-mode fracture surface with indications of transgranular brittle and ductile cracking
from an as-cast state 356 alloy tensile-test specimen. The area of the crack initiation is visible in the center
of (a), and fracture went through the cleavage planes in the silicon particles. In the bottom part of (b), the dendrites of
aluminum solid solution are visible in the shrinkage microarea.

Color Micrographs of Aluminum Alloys with Selective Etching / 525
Table 1 Microetching reagents for examples shown in Fig. 45 through 53

See also the article “Metallography and Microstructures of Aluminum and Its Alloys” in this Volume for discussions on microetchants. Figures 45 through 53 in this atlas are grouped
by etchants in this table.
No. Chemical composition(a) Etching mode Purpose or applicaton Ref
1m 25 mL HNO3 (1.40 M) 70 ⬚C (160 ⬚F), 40 s Phase identification, especially in Al-Cu 1–4
75 mL distilled H2O alloys
2m 20 mL H2SO4 (1.84 M) 70 ⬚C (160 ⬚F), 30 s Phase identification, Al-Cu, Mn, Mg, Fe, 1–5
80 mL distilled H2O 30 s–3 min Be, Ti alloys
3m 1 g NaOH 50 ⬚C (120 ⬚F), 5–15 s Phase identification; 2–4
100 mL distilled H2O Clean in 5% HNO3, rinse in cold water, AlCuMgZn alloys need 2–3 min etching.
prepare fresh before use
1 g NaOH Swab 5–10 s 1
4m 10 g NaOH 70 ⬚C (160 ⬚F), 5 s Phase identification 2, 5
100 mL distilled H2O Prepare fresh before use
5m 0.5 mL HF (40%) At ambient temperature, 5–60 s to alternately Phase identification; 2–8
100 mL distilled H2O polish and etch several times reveals grain boundaries, slip lines in
(The HF concentration can be inreased up to 10 mL). pure Al
Toxic!
6m 5 mL HF (40%) At ambient temperature, 5–60 s Phase identification 2, 5
15 mL HCl (1.19 M)
25 HNO3 (1.40 M)
7m A) 2(4) mL HF (40%) At ambient temperature, 10–30 s Al and Al alloys (Al-Si cast alloys) 3, 4
3(6) mL HCl (1.19 M) Prepare fresh before use
5(10) mL HNO3 (1.40 M)
190 mL distilled H2O (concentration variable)
Toxic!
20 mL reagent 7m Ⳮ 80 mL H2O 5–10 s ... 1
B) 2 mL HF (40%) 10–60 s Form thin layer of etching products on 1
3 mL HCl (1.19 M) Rinse in stream of warm water the specimen surface
20 mL HNO3 (1.40 M)
(Modifed 7m)
8m 0.5–25 g NaOH A few seconds–1 min Al and Al alloys 3
1 g ZnCl2
10m 1 drop HF (40%) 20–25 ⬚C (70–75 ⬚F) Pure Al and Al-Mg, Al-Mg-Si alloys 3
25(30) mL HCl (1.19 M) 10–60 s (etching figures)
25(20) mL HNO3 (1.40 M) Toxic!
25(50) mL CH3OH
11m 2 mL HCl (1.19 M) 10 s All kinds of Al alloys 1
8 mL HNO3 (1.40 M)
45 mL H2O
45 mL CH3OH
12m 10g NaOH 2 min Grain boundaries, Al-Si, Al-Cu alloys 3
5 g K4[Fe(CN)6]
13m 4 g KMnO4 At ambient temperature, 7–45 s Microsegregation in Al alloys 9
Distilled H2O
After dissolution, add 1 g NaOH
14m 4 g KMnO4 Specimen surface must be well polished and Chemical inhomogeneity and 1
2 g Na2CO3 precleaned in 20% H3PO4 at 95 ⬚C (205 ⬚F) microsegregation in Al alloys
94 mL distilled H2O for uniform wettability; after precleaning,
Add a few drops of wetting agent rinse in cold water and immediately
immerse in etchant for 30 s
15m A) 5 mL HF At ambient temperature, a few seconds A) Phase identification 9
95 mL distilled H2O
At boiling temperature, add MoO3 until saturation
B) 10 mL HF B) Grain boundaries revealed
90 mL distilled H2O
At boiling temperature, add MoO3 until saturation
16m 2–2.5 g (NH4)MoO4 Ⳮ 10 mL HNO3 20 ⬚C (70 ⬚F) Phase identification 10
After dissolution, add 190 mL ethyl alcohol (stirring intensively) 30–40 s
17m 1 g (NH4)MoO4 20 ⬚C (70 ⬚F), 30 s–3 min Phase identification in Al-Si alloys 11
200 ml distilled H2O
Add 6 g NH4Cl
(continued)
(a) M, molar concentration
References:
1. Metallography and Microstructures, Vol 9, ASM Handbook, American Society for Metals, 1985, p 351–388
2. M. Orman, Metalografia Aluminium (Metallography of Aluminum), Wyd. Śla˛sk, Katowice, 1957
3. G. Petzow, Metallographisches Atzen, (Metallographic Etching) Gebbruder Borntrager, 1976
4. “Standard Methods for Microetching Metals and Alloys,” E 407-70, ANSI/ASTM, reapproved 1976
5. E. Beraha and B. Shpigler, Color Metallography, American Society for Metals, 1977
6. E. di Russo, The Atlas of Microstructures of Aluminium Casting Alloys, Edimet, Brescia, 1993
7. E. Beraha, Metallographic Reagents Based on Molybdate Solutions, Prakt. Metallogr., Vol 11, 1974, p 271–275
8. R. Poganitsch, R. Sigl, and F. Jeglitsch, Sequential Etching for the Identification of Phases in Technical AlZnMgCu Alloys, Prakt. Metallogr., Vol 21 (No. 5), 1984, p 258–268
9. E. Weck and E. Leistner, Metallographic Instructions for Colour Etching by Immersion, Part III, Deutscher Verlag fur Schweisstechnik-GmbH, 1986
10. M. Richard, Reactif Micrographic pour Colorer le Silicium dans les Alliages d’Al, Fonderie, Vol 28 (No. 326), 1973, p 289–290
11. P. Lienard and C. Pacque, New Metallographic Etching Method for Aluminium Alloys Used in Foundries, The Best of Structure 1–12, Struers, Copenhagen, 1988, p 101–104
12. G. Vander Voort, Ed., Applied Metallography, Van Nostrand Reinhold, 1986

526 / Color Micrographs of Aluminum Alloys with Selective Etching
Table 1 (continued)
No. Chemical composition(a) Etching mode Purpose or application Ref
18m 1–2 g (NH4)HF2 20 ⬚C (70 ⬚F) Phase identification 5, 7
2–3 g Na2MoO4 ⳯ 2H2O 30–60 s
5 mL HCl
19m Stock solution: 20 ⬚C (70 ⬚F) Phase identification 12
3 g (NH4)MoO4 30–40 s
20 mL HNO3
20 mL distilled H2O
Use reagent:
1 p. stock solution Ⳮ 4 p. ethyl alcohol
20m 1.44 g (NH)4NO3 Before use, dilute 1:1 with water, 15–30 s Phase identification 8
9.4 mL HNO3
Add MoO3 in excess
21m 5 mL HCl 30 s All kinds of Al alloys 1
10 mL H2SO4
85 mL distilled H2O
22m 2 g NaOH 2–3 min All kinds of Al alloys 1
5 g NaF
93 mL distilled H2O
23m 5 mL CH3COOH (glacial) 20–30 min All kinds of Al alloys 1
1 mL HNO3 (1.40 M)
94 mL distilled H2O
24m 15.5 mL HNO3 (1.40 M) At ambient temperature, immerse 20–60 s, ag- All kinds of Al alloys 1
0.5 mL HF (48%) itating mildly; second etching in Keller’s
3 g CrO3 reagent may reveal further details of the
84 mL distilled H2O microstructure.
(Graff-Sargent reagent)
25m 200 g CrO3 Pre-etch: 4m, next, 50% HNO3 in water, rinse All kinds of Al alloys 5
20 g Na2SO4 in water, and immediately put in 25m
17 mL HCl (35%)
1000 mL H2O
26m 200 g CrO3 At ambient temperature, 5–30 s All kinds of Al alloys 5
200 g H2SO4
50 g NH4HF2
1000 mL H2O
27m 1–2 mL HNO3 A few seconds–15 min Al-Mg alloys 12
98–99% ethyl alcohol
(a) M, molar concentration
References:
3. G. Petzow, Metallographisches Atzen, (Metallographic Etching) Gebbruder Borntrager, 1976
4. “Standard Methods for Microetching Metals and Alloys,” E 407-70, ANSI/ASTM, reapproved 1976
10. M. Richard, Reactif Micrographic pour Colorer le Silicium dans les Alliages d’Al, Fonderie, Vol 28 (No. 326), 1973, p 289–290

Table 2 Phase identification in aluminum alloys by selective microetching procedure

Results in Fig. 45 through 53 are not always exactly the same as suggested in this table, but results can be considered as comparative examples and a guide for microetch
identification of phase constituents in aluminum alloys.
Si ... Not attacked ... ... Outlined ... Outlined ... Dark blue, Dark blue, ... ... ...
(Ref 1) (Ref 2) (Ref 2) brown 30 s; vio-
(Ref 3) let, 150 s
(Ref 4)
␣-Al ... ... ... ... Grain bound- ... Grain bound- Microse- Grain bound- ... ... ... ...
aries (Ref aries (Ref gregation aries (Ref
1) 1) (Ref 3) 3)
Al9Co2 Not attacked Etched (Ref Dark (Ref 1) Dark (Ref 1) Brown (Ref Brown (Ref ... ... ... ... ... ... ...
(Ref 1) 1) 1) 1)
Al2Cu Red (Ref 1, Not attacked Dark (Ref 1) Dark (Ref 1, Pink (Ref 5) Not attacked ... ... ... Yellow, 30 s Slightly Blue ...
5) (Ref 1) 5) Not attacked (Ref 1) Green 150 s tinted (Ref 9)
Dark (Ref 6) Brown (Ref (Ref 1) (Ref 4) (Ref 7, 8)
7)
Al7(CrFe) Not attacked Not attacked Blue (Ref 1) Blue (Ref 1) Pale brown Not attacked Outlined ... ... ... ... ... ...
Al3Fe ... Black (Ref Dark (Ref 1) Dark (Ref 1, Etched (Ref ... Dark brown ... ... ... ... ... ...
2) 5) 9) dark blue
Etched (Ref Not etched (Ref 6)
10) (Ref 11)
Al3Mg2 Etched (Ref Etched (Ref Not attacked Not attacked Outlined Slightly Outlined ... ... ... ... ... Brown
1) 1) (Ref 1) (Ref 1) (Ref 9) etched (Ref 2) (Ref 9)
Light blue (Ref 1)
(Ref 2)
Slightly
etched
(Ref 1)
Al6Mn Not attacked Not attacked Bright blue Brown (Ref Slightly Not attacked Not attacked ... ... ... ... ... ...
(Ref 1) (Ref 11) (Ref 1) 1) etched (Ref 1) (Ref 2)
(Ref 1)
Al6(MnFe) ... Not attacked Slightly Dark (Ref 1) Dark gray Black (Ref Etched (Ref ... ... ... ... ... ...
(Ref 1) etched (Ref 9) 1) 6)
(Ref 1) Unetched
(Ref 10)
Al3Ni Not attacked Slightly Bright brown Dark (Ref 1), Dark (Ref 1) Brown (Ref Not outlined, ... ... ... Brown ... ...
(Ref 1) etched (Ref 1) outlined 7) darkened (Ref 7, 8)
(Ref 1) brown- (Ref 2)
blue (Ref
2)
Al3Ti Not attacked Not attacked Not attacked Dark (Ref 1) Outlined, Not attacked Light gray ... ... ... ... ... ...
(Ref 1) (Ref 1) (Ref 1) darkened (Ref 1) (Ref 2)
(Ref 2)
CaSi2 ... ... ... ... Dark blue ... Outlined, ... ... ... ... ... ...
(Ref 12) darkened
(Ref 2)
Mg2Si Attacked dis- Etched (Ref Not attacked Brown (Ref Blue (Ref 2, Darkened Blue-brown ... ... ... ... ... ...
soluted 11) (Ref 1) 7) 5) (Ref 7) (Ref 2)
(Ref 5) Darkened Unetched
(Ref 7) (Ref 1)
MgZn2- Etched (Ref Etched (Ref Not attacked Not attacked Outlined Brown (Ref Outlined, ... ... ... ... ... ...
AlCuMg 1) 1) (Ref 1) (Ref 1) (Ref 9, 1) black (Ref
12) 2)
Brown (Ref
2)
Al18Cr2Mg3 Etched (Ref Etched (Ref Not attacked Not attacked Not attacked Not attacked Outlined ... ... ... ... ... ...
1) 1) (Ref 1) (Ref 1) (Ref 1) (Ref 1) (Ref 2)
Al7Cu2Fe Darkened Black (Ref Dark (Ref 1) Dark (Ref 1) Outlined Dark (Ref 1) Not attacked ... ... ... ... ... ...
(Ref 1) 1) (Ref 2) (Ref 2)
Not attacked
(Ref 1)
Al6CuMg4- Dark, red- Black Dark (Ref 1) Dark (Ref 1) Black (Ref Etched (Ref ... ... ... ... ... ... ...
Al2Mg3Zn3 brown 12) 1)
(Ref 1) Etched (Ref
1)
(continued)
References
5. R. Kovacheva, Metallographic Investigation of Al-Si-Mg and Al-Si-Cu Alloys, Prakt. Metallogr., Vol 30 (No. 2), 1993, p 68–77
6. J.R. Davis, Aluminum and Aluminum Alloys, ASM Specialty Handbook, ASM International, 1993
10. J.E. Hatch, Aluminium—Properties and Physical Metallurgy, American Society for Metals, 1984

Table 2 (continued)
A2CuMg Outlined Not attacked Not attacked ... Unetched, Dark (Ref 1, Dark (Ref 2) ... ... ... ... ... ...
(Ref 2) (Ref 1) (Ref 1) gray (Ref 6)
Dark (Ref 12)
10) Black (Ref
2)
Al20Cu2Mn3 Not attacked Not attacked Not attacked Not attacked Brown-blue Not attacked Dark brown ... ... ... Blue ... ...
(Ref 1) (Ref 1) (Ref 1) (Ref 1) (Ref 2) (Ref 1) (Ref 2) (Ref 7)
Not attacked
(Ref 1)
Al7Cu4Ni ... ... Not attacked ... Darkened ... Not attacked ... ... ... ... ... ...
(Ref 1) (Ref 2) (Ref 2)
Al9FeNi Not attacked Not attacked Dark (Ref 1) Dark (Ref 1) Outlined Brown (Ref Outlined, ... ... ... Dark ... ...
(Ref 1) (Ref 1) (Ref 2, 9) 1) darkened (Ref 7, 8)
Dark brown Blue-violet (Ref 2)
(Ref 1) (Ref 7)
b-AlFeSi Slightly Etched (Ref ... Etched (Ref Light brown ... ... ... ... ... Brown-blue ... ...
etched 1, 5) 1, 5) (Ref 5) (Ref 7, 8)
(Ref 5) Dark (Ref 1)
Unetched Darkened
(Ref 1) (Ref 11)
␣-AlFeSi Slightly Slightly Not attacked Not attacked Outlined Not attacked Outlined, ... ... ... ... ... ...
etched etched (Ref 1) (Ref 1) (Ref 2) (Ref 1) darkened
(Ref 1) (Ref 1) Not attacked (Ref 2)
(Ref 1)
␣-AlMnSi Not attacked Not attacked Not attacked Pale brown Outlined Not attacked Outlined ... ... ... ... ... ...
Not attacked
(Ref 1)
␣-AlFeMnSi Slightly Etched (Ref ... ... Light brown ... Brown/1 min Gray (Ref 3) ... ... ... ...
etched 1, 5, 11) (Ref 5) (Ref 2)
(Ref 1, 5) Unetched
(Ref 1)
Al18Mg3Mn2 ... ... ... Not attacked Outlined ... Outlined ... ... ... ... ... ...
(Ref 1) (Ref 2) (Ref 2)
Al5Cu2Mg8Si6 Blue (Ref 5) Dark (Ref 4) ... Dark (Ref 5) Brown-black ... Not attacked ... ... ... ... ... ...
(Ref 2) (Ref 2)
Al8Mg3FeSi2 Brown (Ref Etched (Ref ... Slightly Bright gray, ... Slightly ... ... ... ... ... ...
5) 5) etched outlined etched
(Ref 5) (Ref 5) (Ref 5)
Not attacked
(Ref 2)
References
5. R. Kovacheva, Metallographic Investigation of Al-Si-Mg and Al-Si-Cu Alloys, Prakt. Metallogr., Vol 30 (No. 2), 1993, p 68–77
6. J.R. Davis, Aluminum and Aluminum Alloys, ASM Specialty Handbook, ASM International, 1993
10. J.E. Hatch, Aluminium—Properties and Physical Metallurgy, American Society for Metals, 1984

Color Metallography of Aluminum Alloys / 523
Fig. 41 Lightening effects to enhance contrast between phase constituents in an unetched specimen of Al-Si-Cu-Ni
alloy. (a) Bright-field illumination with silicon (A, dark gray), ␣-Al(FeMn)Si (B, light gray), and Al2Cu (C, beige).
(b) Dark-field illumination with phase boundaries revealed. (c) Cross-pole mode of observation with silicon (dark violet),
␣-Al(FeMn)Si (light violet), and Al2Cu (light pink). (d) Phase contrast with silicon (dark violet), ␣-Al(FeMn)Si (dark pink),
and Al2Cu (pink-yellow with blue contrast on the interfaces). All at 1000⳯. Color version of Fig. 25 in the article “Met-
allography and Microstructures of Aluminum and Its Alloys”

524 / Color Metallography of Aluminum Alloys
Fig. 42 Lightening effects to reveal contrast of crystal orientation in an etched aluminum-copper specimen. (a) Bright-
field illumination with ␣-Al (light gray) and Al2Cu (gray). (b) Dark-field illumination with phase boundaries
revealed. (c) Cross-pole mode of observation revealing Al2Cu crystal orientation in color image. (d) Phase contrast in color
image. All etched with 0.5% HF. All at 200⳯. Color version of Fig. 26 in the article “Metallography and Microstructures
of Aluminum and Its Alloys”
Fig. 44 Phases in an Al-Si-Cu-Ni alloy: Mg2Si (blue

precipitate), Al3NiCu (light-brown precipitate),
Al8Fe(Ni)Mg3Si6 (gray precipitate), ␣-Al matrix (light-gray
Fig. 43 Example of energy-dispersive spectroscopy (EDS)-aided metallography in interpretation of color images in field), and eutectic silicon (dark gray). See Fig. 41 in the
polarized light. The P phase (Al8FeMg3Si6) in an Al-Si-Cu-Ni alloy is indicated by EDS for micrographs with article “Metallography and Microstructures of Aluminum
(a) first position of cross poles and (b) second position of cross poles. Etched with 0.5% HF. 500⳯. Color version of Fig. and Its Alloys” for energy-dispersive spectroscopy plots of
40 in the article “Metallography and Microstructures of Aluminum and Its Alloys” phases. Etched with 0.5% HF. 500⳯.

Fig. 45 Phase constituent identification in various aluminum alloys by means of selective etching with reagent 1m (Table 1). Compare with Table 2. (Małgorzata Warmuzek, Foundry
Research Institute, Kraków, Poland)

Fig. 46 Phase constituent identification in various aluminum alloys by means of selective etching with reagent 2m
(Table 1). Compare with Table 2. (Małgorzata Warmuzek, Foundry Research Institute, Kraków, Poland)


Fig. 47 (continued) Phase constituent identification in various aluminum alloys by means of selective etching
with reagent 3m (Table 1). Compare with Table 2. (Małgorzata Warmuzek, Foundry Research Institute, Kraków,
Poland)



Fig. 49 (continued) Phase constituent identification in various aluminum alloys by means of selective etching with reagent 5m (Table 1). Compare with Table 2. (Małgorzata
Warmuzek, Foundry Research Institute, Kraków, Poland)

Poland)


Fig. 51 Phase constituent identification in alloy 356.0

with reagent 13m (Table 1). Time of attack: 5
s. Orange-green fields are primary dendritic microsegre-
gation regions with ␣-Al (solid solution). Blue fields are in-
terdendritic eutectic (␣-Al Ⳮ Si). 800⳯. Compare with Ta-
ble 2. (Małgorzata Warmuzek, Foundry Research Institute,
Kraków, Poland)
Poland)


with reagent 15m (Table 1). Compare with Table 2. (Małgorzata Warmuzek, Foundry Research Institute, Kra-
ków, Poland)



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ASM Handbook, Volume 9: Metallography and Microstructures Copyright © 2004 ASM International®

G.F. Vander Voort, editor, p711–751 All rights reserved.

Metallographic Techniques for

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Table 3 Characteristics of phase constituents in aluminum-rich aluminum alloys

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Fig. 4 Monophase structure of etched commercially

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Table 4 (continued) example of how microstructures and macros-

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Fig. 17 Effect of phosphorus refinement on the micro-

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Solubility limits, wt%, at:

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Table 11 Reagents for electrolytic polishing and process conditions

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Table 14 Reagents for electrolytic microetching

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Table 15 Applicability of the reagents for chemical microetching, commonly recommended

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Table 16 Microscopic techniques for metallographic examination of the alloy

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Table 18 Phase identification by selective microetching procedure

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Table 22 Reagents used for deep etching of aluminum alloys

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Table 1 Microetching reagents for examples shown in Fig. 45 through 53

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