Inclusions in magnesium and its alloys: a

review
S. Lun Sin, A. Elsayed and C. Ravindran*
High volume application of lightweight materials is the key to improving fuel efficiency and vehicle
performance, and decreasing exhaust emissions to address environmental concerns. Currently,
magnesium alloys, which are the lightest structural materials, represent only y0?3% of an
automobile weight. One of the most important parameters in controlling the properties of
magnesium and its alloys is melt cleanliness, manifested mainly in inclusions. The presence of
such inclusions will strongly influence the mechanical properties and corrosion resistance of
structural components. This paper gives an overview of the current state of knowledge pertaining
to magnesium melt cleanliness. It describes the nature and origin of the inclusions, the methods
for assessing the cleanliness of magnesium, the methods used to control inclusions in the melt
and the relationship between melt cleanliness and the properties of magnesium castings.
Keywords: Magnesium alloys, Inclusions, Melt cleanliness assessment, Melt cleanliness control, Mechanical properties, Fluidity, Corrosion resistance

Introduction negates this benefit. The strength and ductility of Mg

Fuel consumption reduction (and the consequent
reduction in harmful exhaust emissions) is a main
concern of the automobile industry today. Automobile
weight reduction is one of the primary means to achieve
this goal. The observed increase in the use of aluminium
(Al) and its alloys in automobiles is a direct consequence
of the pursuit for weight reduction in the past decades.
Recently, magnesium (Mg) alloys have been consid-
ered as candidate materials to replace Al alloys and
further reduce the vehicle weight, since Mg alloys are
35% lighter than Al (1?74 g cm23 for Mg1 as compared
to 2?74 g cm23 for Al2). Further, Mg alloys exhibit good
damping capacity, high impact resistance and a high
strength to weight ratio. In addition, Mg alloys are
recyclable, thus lessening their impact on the environ-
ment. Magnesium alloys have been implemented in
various applications, specifically in the automotive
industry as shown in Table 1.
Despite these advantages, the average use of Mg in
North American automotive vehicles represents only
0?3% of the total vehicle weight, as shown in Fig. 1.
Comparison of Mg and Al mechanical properties
(Table 2) shows that Mg alloys are at a disadvantage
against Al alloys, as they exhibit lower ultimate tensile
strength (UTS) and yield strength (YS), as well as lower
elastic modulus than Al alloys. The ‘gap’ between Al
and Mg alloys can even be exacerbated if the melt
processing is poor. In particular, the ductility of Mg
alloys can exceed that of Al, and that may be advan-
tageous in some applications, unless melt processing
Centre for Near-Net-Shape Processing of Materials, Ryerson University
101, Gerrard St. E., Toronto, Ont. M5B 2K3, Canada
*Corresponding author, email c.ravindran3@gmail.com
alloys need to be improved, thus rendering them as
viable alternatives to aluminium alloys. Improving the
melt quality or melt cleanliness is key to achieving these
goals.
Ensuring good melt quality involves:
(i) the control of trace elements
(ii) the reduction of dissolved gases in the metal
(iii) the removal of inclusions from the melt.
Variations in the chemical composition of the alloys
and/or in the defect parameters (type, morphology, etc.)
will affect the homogeneity and quality of the final
product in terms of mechanical properties or surface
appearance.10,11
Chemical composition
Since 1922, the melting and the purifying of Mg and its
alloy have had a long development.12,13 It has been
known for years that even trace amounts of iron (Fe),
nickel (Ni), copper (Cu) or cobalt (Co) have deleterious
effects on the corrosion resistance of Mg alloys.14,15 Iron
is the most common impurity which originates from the
steel melting crucibles. Nickel contamination occurs
when high Ni stainless steels are immersed in the Mg
melt (e.g. handling tools or thermocouples). Copper
contamination can arise from Cu bushings in recycled
parts.1 Cobalt may originate from Co based paints,14
but is not a common impurity in Mg alloys and no
tolerance limit has been specified for Co.
These elements have to be removed to ensure
consistent quality of the final product. Minimisation of
these heavy metals in Mg melts can be realised by proper
selection and control of raw materials, alloying addi-
tions procedure, handling/melting tools and equipment
(e.g. use of nickel free low alloy steel crucibles1) and
allowing the impurities to settle to the bottom of the
crucible.16 Iron can be removed through the addition of

ß 2013 Institute of Materials, Minerals and Mining and ASM International

Published by Maney for the Institute and ASM International
DOI 10.1179/1743280413Y.0000000017 International Materials Reviews 2013 VOL 58 NO 7 419
Lun Sin et al. Inclusions in magnesium and its alloys

1 Vehicle materials distribution for a 1500 kg (average) North American vehicle5

manganese to molten Mg. The melt is then cooled,
resulting in the precipitation of Fe–Mn–Al intermetallic.
Control of melt temperature is thus crucial.
Hydrogen
Hydrogen solubility is greater in the liquid than in the
solid state for Al and Mg alloys. For Al, the maximum
solubility of hydrogen in the liquid and the solid near the
melting point are 0?65 cm3/100 g and 0?034 cm3/100 g
respectively. For Mg, they are 27 cm3/100 g and 19 cm3/
100 g respectively.17 The solubility of hydrogen in
molten Mg is significantly higher than in Al. However,
molten Mg saturated with hydrogen rejects only 32% of
hydrogen during solidification as compared to alumi-
nium that rejects 95%.14 If the concentration of
hydrogen is above the maximum solid solubility,

Table 1 Magnesium casting alloys: properties and automotive applications3,4

Alloy family Mg–Al–Zn Mg–Al–Mn Mg–Al–Si Mg–Al–RE* Mg–Al–Sr/Ca

Typical AZ91D AM60B, AM50A AM20 AS41, AE42, AJ52, AJ62,

alloys AS21 AE44 AXJ530,
MRI 153M,
MRI 230D
Properties Excellent castability Excellent ductility High ductility and Good strength
and good strength and energy impact strength and good creep
absorbing properties resistance up to
about 150uC
Applications Steering column Automobile seat Automotive safety parts, High temperature
brackets, cylinder frames, steering seat frames applications (e.g.
block, transmission wheel, instrument engine cradle,
case panel, brackets powertrain components)
*RE denotes rare earth elements.
Table 2 Comparison of typical properties of common Mg and Al automotive alloys*1–3,5–9

Tensile properties Tensile properties

at 20uC at 150uC Elastic % Tensile creep
Density/ modulus/ at 50 MPa, 200 h,
Alloy g cm23 UTS/MPa YS/MPa Elongation/% UTS/MPa YS/MPa Elongation/% GPa 150uC

A380-F 2.76 324 160 4.0 227 145 10.0 71.0 0.08
319.0-T6 2.79 248 165 2.0 N/A N/A N/A 74.0 N/A
332.0-T5 2.76 248 193 1.0 214 165 2.0 77.0 N/A
Al 356.0-T6 2.68 262 186 5.0 145 117 10.0 72.4 N/A
A356.0-T61 2.69 283 207 10.0 145 117 20.0 72.4 N/A
383.0-F 2.74 310 150 3.5 N/A N/A N/A 71.0 N/A
390.0-T5 2.73 296 265 1.0 N/A N/A N/A 81.2 N/A
AZ91D 1.81 250 160 7.0 169 105 16.0 45.0 2.7
AM60B 1.80 240 130 13 N/A N/A N/A 45.0 N/A
AM50A 1.77 230 125 15 N/A N/A N/A 45.0 N/A
Mg AM20 1.75 210 90 20 N/A N/A N/A 45.0 N/A
AS41 1.77 240 140 15 153 94 17 45.0 0.05
AS21 1.76 220 120 13 130 87 20 45.0 0.19
AE42 1.79 230 145 11 140 88 23 45.0 0.06
*All die cast, except 319?0-T6, 332?0-T5, 356?0-T6 and A356?0-T61 (permanent mould).
N/A: none available.

420 International Materials Reviews 2013 VOL 58 NO 7


formation of pores can occur upon solidification.2 This
represents a serious problem as porosity affects the
mechanical properties and the surface quality of
castings. The acceptable hydrogen levels for Al and
Mg alloys are 0?1 cm3/100 g or lower18 and 15–20 cm3/
100 g,4,19 respectively. The level of hydrogen can be
reduced by bubbling chlorine or an inert gas through the
melt.12,20
There is no commercial instrument available to
measure hydrogen content in Mg melts. Researchers
have utilised different techniques (e.g. helium bubbling,
vacuum extraction, complete combustion of a Mg
sample)21 to measure hydrogen concentrations, some-
times making the results difficult to compare and
unreliable.22
Inclusions
Unlike Al alloys, Mg alloys form a loose, permeable film
which does not protect the molten metal from further
oxidation. Consequently, molten magnesium will oxidise
and burn rapidly in contact with air if special precau-
tions are not taken (e.g. use of flux, cover gas or alloying
additions such as beryllium).1 The high oxidation
potential of Mg usually results in inclusion contents
10–20 times higher than that of Al (0?1–10 ppm for pure
Al, 10–200 ppm for pure Mg).23 Inclusions in Mg alloys
reduce mechanical properties, are detrimental to surface
finish, increase porosity and exhibit a tendency to
increase corrosion.24,25
The maximum allowable concentrations of the major
impurities in Mg alloys and the methods to remove them
are summarised in Table 3.
There is a need to understand and control all aspects
of metal handling and processing to improve the
consistency of quality and properties of the cast product.
This also applies to Mg recycling, for which the large
amount of scrap runners, overflows, flash and rejected
castings from Mg die casting processes requires careful
control of melt practices to ensure metal quality.29,30
Many efforts have been devoted to improve and assess
the melt cleanliness of Al alloys. In comparison, limited
information is available for Mg alloys. The techniques
used for Al were generally applied to Mg. However, due
to the reactive nature of Mg, the adaptability and
applicability of these techniques to Mg melts can be
challenging. This review paper is written with a focus on
the characterisation and formation of inclusions within
Table 3 Impurity levels in Mg alloys
Impurity Typical level
Dissolved elements
Fe 200–400 ppm14
Ni Solubility in Mg at 650uC: 32 wt-%1
Cu Solubility in Mg at 650uC: 70 wt-%1
Hydrogen In pure Mg: up to 24 cm3/100 g
of metal21
In AZ91 alloy (between 650 and
750uC): 6–14 cm3/100 g27
Inclusions Variable (depends on processing
conditions)
Lun Sin et al. Inclusions in magnesium and its alloys
Mg melts and covers their assessment, control and
effects on properties of the alloys.
Inclusions in magnesium alloys
Characterisation of inclusions in magnesium
alloys
Inclusions present in molten Mg can be categorised into
two major groups:31
(i) non-metallic inclusions: these include oxides and
nitrides; sodium, magnesium and potassium
based chlorides; aluminium and calcium based
carbides, magnesium based sulphides (MgS),
fluorides (MgF2) and sulphates (MgSO4).
Oxides are the most predominant non-metallic
inclusions, followed by nitrides
(ii) intermetallic inclusions: these include iron rich
intermetallic phases, which precipitate during
iron removal. Almost all intermetallic inclusions
contain iron.
Both inclusion types are potentially harmful to the
properties of Mg alloys, in particular tensile strength,
elongation and corrosion resistance. Further, descrip-
tion of the influence of inclusions on the properties of
Mg alloys is discussed in the section on ‘Effect of
inclusions on properties of magnesium alloys’. The
characteristics of the various inclusions found in Mg
alloys are summarised in Table 4, and the typical
inclusions are shown in Fig. 2.
Origin of inclusions in magnesium alloys
Reaction with air
During the melting process, molten Mg reacts with
oxygen to form magnesium oxide (MgO) when the melt
is exposed to the atmosphere.31,35 Molten Mg can also
react with the moisture in air to form MgO and
hydrogen, which can result in a fire or explosion.
Therefore, all tools to be used must be dry/preheated
before immersion in the melt. Water should not be used
to fight magnesium fires.1 The casting process, depend-
ing on the pouring technique and gating design, almost
always leads to some melt turbulence, which entraps
inclusions and exposes a fresh melt surface to the
atmosphere, further increasing the number of inclusions
in the melt. Stirring, charging, ladling, poor venting,
removal of dross and sludge and excessive movement of
the mould before solidification is complete12 also
Acceptable levels Methods for achieving acceptable limits
0.0035–0.004 ppm26 Addition of Mn and Al additions to form
Al–Fe–Mn phases14
0.001–0.01 ppm26 Dilution, addition of Al and Zr to reduce
Cu solubility in Mg and promote formation
of AlNi precipitates14
0.008–0.25 ppm26 Dilution, removed alongside Fe in Al–Fe–Mn
phase formation14
15–20 cm3/100 g4,19 Gas bubbling (chlorine or inert gas) through
the melt12,18
Less than 500 ppm28 Addition of flux or fluxless refining (protective
atmospheres, filtration, inert gas bubbling,
melt sedimentation, ultrasonic purification,
electromagnetic separation)
International Materials Reviews 2013 VOL 58 NO 7 421
Lun Sin et al. Inclusions in magnesium and its alloys

2 Optical micrographs of a an oxide cluster in AZ91 alloy, b a ‘snaky’ oxide in AM50 alloy and c Mn–Al particles in
AM60 alloy34

promote the entrapment of oxides. Oxide defects exhibit
various morphologies, from particles to films. The oxide
films can measure up to 50 mm in length with a thickness
of 0?5 mm. The oxide particles are commonly seen as
clusters less than 50 mm in diameter. Both oxide films
and clusters have high surface to volume ratios and
cannot be removed by melt settling.35
Magnesium nitrides (Mg3N2), which form as a result
of the reaction of Mg with nitrogen, may appear
together with oxide clusters. As can be seen in Table 5,
the Gibbs free energy associated with the oxidation of
magnesium is more negative than the Gibbs free energy
associated with the formation of magnesium nitride,
meaning that Mg preferentially reacts with oxygen over
nitrogen. Magnesium nitride will not form unless the
partial pressure of oxygen becomes extremely low.35
There is no indication that nitride inclusions appear
independently of oxide inclusions.
Reactions with fluxes
Fluxes are used to protect magnesium melts from
oxidation and for refining (removal of inclusions).
Flux inclusions (e.g. MgCl2, CaCl2) occur if unabsorbed
protective flux remains on the metal surface, the flux is
not viscous enough, there is brittle or powdery flux due
to long handling, pouring is too fast or if there is
incomplete removal of the flux adhering to the lip of the
pot before pouring.38 Magnesium chloride in the flux

Table 4 Inclusions in magnesium alloys17,32,33

Type Morphology Dimensions/mm Density/g cm23

Oxides
MgO Particles 10–300 3.58
Films 0.5–1 (thickness)
50–400 (length)
MgO.Al2O3 (spinel) Particles 3.58
Nitrides
Mg3N2 Particles 10–300 2.71
Films 0.5–1 (thickness)
50–400 (length)
Carbides
Al4C3 Particles 0.1–10 2.36
CaC2 Particles 2–20 2.22
Chlorides and salts
MgCl2 2.32
NaCl Particles 10–50 2.17
CaCl2 2.15
KCl 1.98
Other non-metallic inclusions
Fluorides (MgF2) 3.15
Sulphides (MgS) Particles 2.68
Sulphates (MgSO4) 2.66
Borides (FeB) 7.15
Iron rich intermetallic compound
Al8(Mn,Fe)5, a-AlMnFe, (Mn,Fe)5Si3, Particles, needles ,20 4–7
Al8(Mn,Fe)4RE, a-Fe, Fe2(Si,B),
Fe3(Al,Si), (Fe,Mn)3Si

Table 5 Standard Gibbs free energy DGreaction as function of temperature T of selected reactions36,37

DGreaction (kJ mol21)5azbTlog TzcT

Reaction a b c Temperature range/K

Mg(l)zKO2(g)5MgO(s) 2608 21.00 0.1128 923–1380

Mg(l)zMN2(g)51/3Mg3N2(s) 2162 0 0.0757 923–1061

422 International Materials Reviews 2013 VOL 58 NO 7


can react with oxygen and water in the air to form MgO,
which can become entrapped in the casting.39 Similarly,
the use of boride containing fluxes could lead to the
formation of FeB inclusions.40 Considerations related to
flux entrapment and melt loss41 led to a shift to the use
of protective atmospheres.42
Reactions with protective gases
Protective atmospheres43–52 are used to prevent oxida-
tion or burning of molten Mg and consequently to
reduce the formation of inclusions in the melt. Some
cover gases, including sulphur dioxide (SO2), sulphur
hexafluoride (SF6), hydrofluorocarbons (HFC) and
fluorinated ketones (FK), modify the natural oxide film
such that Mg vaporisation is suppressed and reactive
gases are excluded. For example, sulphur dioxide reacts
with Mg to form MgSO4, MgO or MgS.46 With SF6,
HFC and FK, the reaction products are MgO and
MgF2.43–45,47–52 All these compounds can enter the melt
and lead to the formation of inclusions. Although
protective gases may lead to the formation of inclusions,
their absence would be more detrimental to the proper-
ties of Mg alloys. Proper melting, handling and pouring
procedures should minimise their formation.
Reactions during melt treatment and alloying
Inclusions can be introduced during the process of
iron removal using manganese. With the addition of
manganese, intermetallic particles containing iron,
manganese and aluminium form.31 Inclusions can also
result from degassing and grain refinement by the addi-
tion of hexachloroethane (C2Cl6), calcium cyanamide
(CaNCN) or by the addition of alloying elements (e.g.
Al4C3 in Mg alloyed with Al).31
Reactions during casting
During casting, poor running system design is generally
associated with high surface turbulence and greater
entrainment of oxide films. The entrained oxides are
typically double oxide film defects (bifilms) comprised of
folded MgO films.53,54 The high reactivity of Mg results
in rapid formation of MgO films during pouring that
quickly thickens to produce a tube of oxide that
surrounds the falling metal stream. This tube of oxide
is not in danger of becoming entrapped within the liquid
metal if the oxide film is unbroken. A similar phenom-
enon occurs in Al alloys and is due to the same
mechanism of rapid thickening of oxide films.18 The
oxide film forming at the surface of the Al melt is
relatively thin and elastic as compared to the thick and
cracked oxide film forming at the surface of the Mg
melt. As a result, Mg alloys may be more prone to bifilm
formation than Al alloys.
Inclusions can also be generated during die casting
from oxidation in the shot sleeve, entrapment of air
during casting and absorption of lubricants spread on
the die surface.1,11,14,31 In sand casting, turbulent flow
may cause sand grains to detach from the mould wall
and be entrained within the Mg melt, with which they
react. The inclusions formed are called ‘reacted sand
inclusions’.14,31,55
Assessment of cleanliness of
magnesium melts
A summary of the methods used or considered to assess
the metal cleanliness in the Mg industry is shown in
Lun Sin et al. Inclusions in magnesium and its alloys
Table 6, but none of these methods is considered as a
standard for determining Mg melt cleanliness.
Metallographic techniques
Classic metallographic techniques
Classic metallographic techniques involve the examina-
tion of ingot slices to determine the presence of
inclusions. It allows the determination of inclusion
amount, size, shape and distribution. Metallographic
analysis can be combined with image analysis to
determine the particle size, number of particles, percen-
tage of oxide in the sample, or with scanning electron
microscopy (SEM) and energy dispersive X-ray spectro-
scopy (EDS) to determine the nature of the inclusions
and the possible source of melt contamination.56
However, optical metallography requires multiple steps:
sectioning, grinding, polishing and examination. The
technique is therefore time consuming and expensive.
Also, the sample size is relatively small, possibly leading
to results which are non-representative of the sample.
Humidity test
The humidity test is used in the industry to detect and
identify flux inclusions in Mg alloys. The surface to be
examined is carefully ground and polished. The pre-
pared specimens are then placed in a chamber where
humidity conditions are controlled (e.g. 95% relative
humidity at 38uC1). Corrosion occurs at the site of
certain inclusions, others being relatively unaffected.
The corrosion products are then examined by micro-
chemical techniques to identify the inclusions.22
However, the results are available only after sufficient
corrosion on the sample has occurred which can
typically take 24–48 h. Fracture ingot surfaces are
sometimes exposed to high humidity in a humidity
chamber. Salt inclusions pick up moisture and bloom,
indicating the presence of fluorides and chlorides.75
Techniques based on filtration of liquid metal
Hydro magnesium inclusion assessment method (HMIAM)
In the hydro magnesium inclusion assessment method
(HMIAM) or vacuum filtration technique, a known
volume of melt is drawn through a stainless steel filter by
vacuum. The inclusions are retained on top or within the
filter (Fig. 3). Upon solidification and cooling, the filter
and its contents are sectioned parallel to the flow
direction and examined using an optical microscope.
The amount of inclusions is determined in terms of
volume of particles per unit weight of metal drawn
through the filter. The major advantage of HMIAM is
that sampling is performed directly in the melt.31,35
However, this method can be considered too time
consuming.57 The quantity and morphology of oxides
in ingots or die cast components may also be different
from those observed on the filter due to different
solidification conditions (e.g. melt temperature).58
Pressure filtration technique: PoDFA and Prefil
Both PoDFA (porous disc filtration analysis) and Prefil
techniques involve forcing a known amount of molten
metal under pressure through a filter. In the PoDFA
method (Fig. 4), the inclusions concentrated inside or on
top of the filter are examined metallographically in terms
of size, colour and morphology.31,35 In the Prefil test, the
flow rate of molten metal through the filter is measured
and used as an indication of the melt quality: clean
International Materials Reviews 2013 VOL 58 NO 7 423
Lun Sin et al. Inclusions in magnesium and its alloys

metals will flow quickly, whereas inclusions in molten
melts build up on the filter surface and reduce the
flowrate. These two methods have been applied to
measure the melt quality of Al melts, but it was only
recently that they were adapted to Mg melts.59
Self-gravitation filtering technique
In the self-gravitation filtering technique, specifically
designed for Mg alloys, a filter tube containing two
sintered metal fibre filter discs is immersed in the melt,
allowed to be preheated for 3–4 min and then lifted up
out of the melt at a constant speed. As the tube rises, the
metal flows through the filters by self-gravitation. The
filter cake thickness is correlated to the inclusion
content, thereby obtaining an estimation of the melt
cleanliness. The inclusions collected on the filter discs
can be subsequently analysed by optical microscopy.60
The technique is still under development to enable the
monitoring of the filtration rate.
Techniques based on melt centrifugation and
sedimentation
This technique is based on the separation of phases with
different densities. The samples are heated to 720–
800uC, held isothermally for 5 min and then centrifuged
at high speed (200–2500 rev min21) until the melt
solidifies. The temperature is measured continuously
with a thermocouple located below the crucible.61
During this period, inclusions are sedimented at the
bottom of the crucible. The inclusions are subsequently
analysed using optical microscopy. Experimental results
showed that (Fe,Mn)3Si particles present in Mg melt

Table 6 Methods for metal cleanliness assessment used or considered for use in magnesium industry*

Method Response time Information Detection limits Sample size Cost References

Metallographic Hours/days Qualitative/total 1–2 mm about 256 Low/moderate 56

techniques particle content 25 mm
Humidity test Days Qualitative/detection about 256 Low/moderate 22
of salt inclusions 25 mm
HMIAM (Hydro Hours/days Qualitative/total 1–2 mm/y4 0.4–1.9 kg Low/moderate 31, 35, 57, 58
Magnesium), content each type, ppm
OM/OM-IAS/ NSD each type
SEM-EDS
PoDFA/Prefil Hours/days Qualitative/total 20–50 mm 2 kg Low/moderate 31, 35, 59
content each type,
NSD each type
Self-gravitation Hours/days Qualitative/total Variable Low/moderate 60
filtering technique content each type,
NSD each type
Melt centrifugation Hours/days Qualitative/total 1–2 mm/10– 50 g Low/moderate 61
and sedimentation content each type, 100 ppm
NSD each type
K-mould Minutes Relative total 0.1–1% Fractures Low 31, 35, 53
inclusion contents
Light reflectance Seconds/ Total particle 0.2%MgO Fractures Low 35, 55, 58, 62
technique minutes content
GD-MS/AES Minutes/hours Total oxide 0.1–1 ppm y1 g High 35, 58
FNAA Minutes/hours Total oxide 1–10 ppm 5–30 g High 56, 63, 64
ASES Minutes/hours Total oxide 200 ppm y1 g High 63
LIBS Minutes Qualitative and 3 mm Variable Moderate 65
quantitative/mapping
Matrix dissolution: Days/weeks Qualitative/total 1–2 mm ,100 g Low/moderate 35,66
OM/SEM–EDS contents each type,
NSD each type
Radiography Hours Quantitative Magnesium oxide: Variable Moderate/high 1
thickness equal to
about 10% of the
thickness being
examined Flux
inclusions: 2%
LiMCA Online NSD, total 10–20 mm … Moderate/high 31, 35, 67, 68
non-conductive
particles.
LECOH oxygen and Minutes/hours Total oxide 0.1–1 ppm y1 g High 35, 69
nitrogen
determinator
Ultrasound Online NSD, total contents y100 mm … Moderate/high 31, 70, 71
Conductivity Minutes/hours Total non-conductive 0.1% 1–10 g Low 72
measurement particles
X-ray tomography Minutes/hours Quantitative/size About 1–3 mm Variable/ High 73, 74
distribution, synchrotron:
inclusion 1 mm3
morphology (3D)
*OM: optical microscopy; SEM: scanning electron microscopy; EDS: energy dispersive X-ray spectroscopy; IAS: image analysis
systems; GD: glow discharge; MS: mass spectroscopy; AES: atomic emission spectroscopy; FNAA: fast neutron activation analysis;
ASES: arc spark emission spectroscopy; LIBS: laser induced breakdown spectroscopy; LiMCA: liquid metal cleanliness analyser;
NSD: number size distributions; PoDFA: porous disc filtration analysis.

424 International Materials Reviews 2013 VOL 58 NO 7

 Lun Sin et al. Inclusions in magnesium and its alloys

3 Schematic of the hydro magnesium inclusion assessment method3

could be analysed by this technique. However, the

method can only be used for particles larger than 2–
4 mm in diameter. Further, this technique is time
consuming and oxides and nitrides in Mg alloys are
difficult to analyse.

Fracture surface examination

Generally, there are more inclusions visible on a
fractured surface, as fracture often propagates along
inclusions. Fractography is thus a quick and simple
method used to assess melt cleanliness. Specific methods
based on fracture surface examination have been
developed and presented in the following sections.
K-mould method
In the K-mould method, a flat plate casting with four
cast-in knife edge notches is produced. The notches serve
as fracture points (Fig. 5).31,35 The design of the knife
edges in the mould enhances the efficiency of capturing
the inclusions on the fracture faces. Multiple samples of
the plates are cast and fractured immediately after
solidification. The fracture surfaces are examined
visually for inclusions. The inclusion level is expressed
5 K-mould method31
as the number of defects seen per number of fracture
surfaces examined.
The K-mould is a simple shop floor test for detecting
inclusions. The main advantages of this technique
include quick results, minimal cost, low required level
of operator skill, sampling flexibility and sample
retention.77 However, the volume of metal examined is
relatively small and only large inclusions in the size
range of 60–80 mm can be discerned easily with this
method.31,78

4 Schematic of the pressure filtration technique76

International Materials Reviews 2013 VOL 58 NO 7 425

Lun Sin et al. Inclusions in magnesium and its alloys
Light reflectance technique
The light reflectance technique is based on the differ-
ences in optical characteristics between Mg and magne-
sium oxide. A gravity cast sample is fractured and the
fracture surface is placed in the aperture of a brighti-
meter. The sample is illuminated at a 45u angle and the
intensity of the reflected light is measured (Fig. 6). If
inclusions are present in the material, the incident light
will be scattered at the surface of the specimen due to
multiple reflections and refractions. This interaction is
called diffuse reflectance. In Mg alloys, magnesium
oxide inclusions absorb more light than the matrix, and
as a result, the reflectance of the specimen is reduced.
The reflectance should therefore correlate with the oxide
inclusion content in the specimen.62,79 However, this
technique exhibits high detection limits (y0?2%)35,58,62
and cannot distinguish between different inclusion types
and sizes.35,58
Compositional analysis
Spectroscopic methods
Fast neutron activation analysis (FNAA), glow dis-
charge mass spectroscopy (GD-MS) and glow discharge
atomic emission spectroscopy (GD-AES) have been
used to determine the chemical composition of Mg
melts.
In the FNAA method, the samples are irradiated with
14?8 MeV neutrons and the reaction product (16N) is
detected. The number of 16N atoms detected directly
corresponds to the number of oxygen atoms in the
sample.56,63,64
In glow discharge source techniques, the sample is
exposed to an argon plasma which uniformly erodes
material from the sample surface. The sputtered atoms
are ionised in this plasma and extracted into a mass
spectrometer for separation and detection in GD-MS. In
the case of GD-AES, a spectrometer is used to measure
the wavelength and intensity of the light emitted by the
sputtered atoms when they return to the ground
electronic state.
FNAA, GD-MS and GD-AES have low detection
limits (0?1–10 ppm) and high accuracy (5–20%).
However, these methods all involve sample preparation,
are time consuming, and require sophisticated and
expensive instrumentation.35,58 In addition, the FNAA
method requires a neutron source such as a nuclear
reactor, which usually is not accessible. Also, there is no
industry specification for acceptable levels of oxygen in
the samples and there is no exact correlation between the
oxygen content within the sample and the oxide
content.35,58 Finally, these methods do not provide
information on the inclusion size and morphology.
In arc spark emission spectroscopy, a voltage arc at
the surface of the sample forms a plasma and the
radiated light is collected and analysed. However,
wavelength limitations make the measurement of oxygen
difficult. Also, the sensitivity is limited to about
200 ppm. Finally, since the sample analysed is relatively
small, the results may not be representative.63
Laser induced breakdown spectroscopy (LIBS) has
recently shown a potential for rapid qualitative and
quantitative chemical analysis of various materials.65
This technique is characterised by its rapidity, non-
contact optical nature and its absence of sample
preparation and is suitable for online measurements. It
426 International Materials Reviews 2013 VOL 58
6 Schematic diagram of the light reflectance unit62
uses the light emitted from a laser generated plasma to
determine the composition of a sample. Figure 7a shows
a map of oxygen in a Mg sample obtained by LIBS.
Comparison with an optical micrograph (Fig. 7b)
revealed that the darker feature seen in LIBS mapping
corresponded to oxide inclusions. LIBS can thus be
applied to locate inclusions in Mg samples.
Matrix dissolution technique
In the matrix dissolution technique, the metal sample is
dissolved in acid, bromethanol or methanol, leaving a
residue of inclusions. The dissolution of a suitable sized
sample (e.g. 30 g) takes up to 1 week. Inclusions are
measured and quantified by means of optical micro-
scopy, SEM/EDS, X-ray fluorescence or Coulter
Counter technique.35,66
In recent years, a method for Mg melt cleanliness
assessment, based on wet chemistry, was developed
(MagOxide).58 It allows the quantification of MgO and
Al–Mn intermetallics in pure Mg and Mg alloys. It is
based on chemical dissolution of the Mg matrix and
subsequent analysis of MgO residues by inductively
coupled plasma emission spectrometer. However, the
samples are only 2–3 g and may not be representative of
the whole melt.
Other methods
Radiography
Radiography can be used to detect inclusions in Mg
alloys, based on the difference in X-ray absorption
between the Mg matrix and the defects. However, the
difference in the absorption coefficient between Mg and
its oxide is relatively small. As a result, an oxide skin is
very difficult to detect. Also, only oxide inclusions
having a minimum thickness equal to about 10% of the
sample thickness can be detected. For flux inclusions,
the detection limit is approximately 2%.1
Liquid metal cleanliness analyser (LiMCA)
The LiMCA instrument offers on-line measurement of
non-conducting particles. The LiMCA technique was
developed based on the electric sensing zone principle. A
schematic of the LiMCA instrument is shown in Fig. 8.
The unit includes a probe, current source and signal
processing system. The probe consists of two electrodes
and an electrically insulating sampling tube with an
orifice through its surface. Molten metal is drawn
through the aperture in the presence of a large DC
NO 7
 Lun Sin et al. Inclusions in magnesium and its alloys

7 a LIBS mapping of oxide inclusions in magnesium samples and b corresponding optical micrograph65

current. Non-conducting inclusions in the melt are
detected by measurement of the change in the electrical
conductivity as they pass through the aperture.31,35,67,68
The LiMCA technique can be made available online
very quickly at time intervals on the order of 1 min and
is able to detect inclusions as small as 20 mm. However,
this method presents several disadvantages: (1) it cannot
detect conductive inclusions such as intermetallic
particles, which are present in molten Mg; (2) the orifice
can be blocked by large size inclusions; (3) the amount
of molten metal that the LiMCA can assess at a time is
very limited; (4) it fails to provide information on the
chemistry, shape or the physical state of the inclusions;
(5) there are difficulties in finding appropriate non-
conductive materials for sampling tubes that are also
non-reactive with Mg alloys; and (6) the cost is very
high.31
LECO method
The LECO method (oxygen and nitrogen determinator)
may be applicable for detecting total oxygen and nitrogen
in solid Mg samples. The method is based on fusion of a
solid metal specimen in a graphite crucible. At high
temperatures (up to 2300uC), magnesium oxide will be
reduced to magnesium and carbon monoxide (CO) in the
presence of carbon. The amount of CO developed can be
quantified and related to the original MgO content.69 The
detection limit is claimed to be 0?1 ppm for both oxygen
and nitrogen.35 Large inclusions may affect the results, as
the sample size is only about 1 g.

8 Schematic of the liquid metal cleanliness analyser technique78

International Materials Reviews 2013 VOL 58 NO 7 427

Lun Sin et al. Inclusions in magnesium and its alloys
9 Schematic of an ultrasonic apparatus (UT: ultrasonic
transducer)70
Ultrasonic methods
Ultrasonic methods have been reported as online
methods to monitor molten metal properties.31 A
schematic of an ultrasonic apparatus is shown in
Fig. 9. During measurement, a signal is sent through
the melt by a transmitter and collected by a receiver. If
there is no inclusion, the signal will propagate in the melt
without much attenuation. However, the signal energy
will be reduced when it is reflected at inclusions.
Experimental results show that it is possible to use
ultrasound to measure oxide content in molten Mg. This
technique is capable of detecting both non-metallic and
intermetallic inclusions. However, only inclusions larger
than 100 mm are detectable due to limitations in sound
frequencies generated by piezoelectric crystals.31,70
Substantial development is still needed to implement
this technique for Mg alloys.
Chen and Wei71 proposed an ultrasonic vibration
method for the diagnosis of oxide films entrapped in cast
Mg alloys. The method is based on the phenomena of
acoustic cavitation. A polished solid Mg sample is
placed inside an ultrasonic cleaner filled with water. The
ultrasonic sound waves generate cavitation bubbles,
which in turn can produce microjets and shock waves
and erode the surface of the sample. Oxide films then
become visible as foggy marks on the surface of the
sample.
Conductivity measurement
Electrical conductivity measurements are a fast and
sensitive means of non-destructive evaluation that offers
the potential of detecting the electrically insulating oxide
particles embedded in the conductive Mg matrix.72
However, it was found that electrical conductivity was
very sensitive to the Al level and the amount of porosity
in Mg alloys. As a result, electrical conductivity
measurement cannot be used to measure the inclusion
level in Mg samples.
X-ray tomography
X-ray computed tomography is a non-destructive
technique which can be used to obtain 3D information
on a sample structure, e.g. the size, shape, connectivity
and spatial relationship between the inclusions in the
castings.73 X-ray computed tomography uses X-ray
tubes,73 although a synchrotron can also be used as a
428 International Materials Reviews 2013 VOL 58 NO
X-ray source.74 Inclusions and precipitates in Mg alloys
appear as regions of darker contrast than the Mg matrix
with rod-, plate- and flake-like morphologies.74 The
limitations of this technique are its relatively high cost,
long processing times and, if applicable, limited acces-
sibility to a synchrotron.
Control of inclusions in magnesium
alloys
Inclusions can be minimised by the application of best
practices in the foundry. These include strict attention to
charge selection, melting conditions, careful skimming
of slag or dross, development and improvement of
gating system design to minimise turbulence and process
control (e.g. temperature control to minimise the
precipitation of intermetallic particles and good settling
practice). The inclusion content in the melt can be
further decreased by refining techniques (cleaning or
separation of nonmetallic inclusions from the melt) or
alloying additions. These are described in the following
sections.
Addition of flux
In flux based refining, the melt is heated to approxi-
mately 705uC, a flux is added and the melt is stirred
thoroughly. The flux absorbs the oxides present in the
melt to produce a sludge. After stirring, the sludge is
allowed to settle to the bottom of the crucible, thereby
enabling the refined melt to be separated from the
sludge. Typical fluxes used in Mg refining are composed
of magnesium chloride MgCl2, other chlorides (e.g.
potassium chloride KCl, sodium chloride NaCl) and
calcium fluoride CaF2.1 Recently developed fluxes can
also contain up to 30 wt-%TiO2. The added TiO2
facilitates Fe removal in melts by forming Ti–Fe
compounds that settle at the bottom of the crucible.30
The actual composition of the flux, however, will
depend to a large extent on the type of Mg alloy to be
refined. The Gibbs free energy of formation for some
chlorides is shown in Fig. 10.
The major alloying elements (Al, Zn, Mn) are stable
in the melt.14,41 However, it can be seen that strontium
chloride SrCl2, calcium chloride CaCl2 and chlorides
containing rare earth elements RE (YCl3, CeCl3, GdCl3)
are more stable than MgCl2. This indicates that the
magnesium chloride in the flux should react with Sr, Ca
and rare earth elements, resulting in the loss of these
elements. The reactions are shown below:
SrzMgCl2 ?MgzSrCl2 (1)
CazMgCl2 ?MgzCaCl2 (2)
REzMgCl2 ?Mgz RECl3 (3)
In order to solve this problem, two approaches were
considered. In the first one, fluxes were specially for-
mulated to minimise the loss of rare earth elements.81–86
The second approach consisted of using fluxless refining.87
Fluxless refining
Flux free refining includes all refining processes where
salt is not used. Inclusions are removed from the bulk
melt and transferred either to the melt surface, settle to
the bottom or stick to the crucible walls before casting.69
7

10 Standard Gibbs free energy of formation of some chlorides.22,80 Approximation: DG05DH0–TDS0
Fluxless refining processes are based on sedimentation
(settling), floatation, interception or electromagnetic
forces.
Protective atmospheres
Protective atmospheres43–52 are used to prevent oxida-
tion or burning of molten Mg and consequently to
reduce the formation of inclusions in the melt. There are
two types of protective gas atmospheres:88 non-reactive
gases and oxide film modifiers.
Non-reactive gases, such as nitrogen and argon,
prevent burning. However, use of such gases is
impractical outside of the laboratory as they do not
suppress Mg vaporisation which can result in melt loss.
In addition, as Mg vaporises, it condenses into
pyrophoric size particles on the cooler surfaces of the
furnace.39
The other method of melt protection involves the use of
a gas which modifies the magnesium oxide film forming
naturally on the surface of the melt, thereby suppressing
vaporisation. Since the 1970s, the Mg industry has largely
used sulphur hexafluoride (SF6) to protect Mg
melts.39,43,44,51,88–93 Sulphur hexafluoride is an effective
cover gas due to its ability to form a dense film containing
Mg oxide (MgO) and Mg fluoride (MgF2) on the molten
Mg surface. This film prevents further oxidation and
evaporation of Mg.43,44,93 Sulphur hexafluoride is also
attractive as a cover gas since it is odourless, colourless,
non-toxic, non-flammable and non-corrosive. It has been
found that a combination of SF6 and CO2 is better than
SF6 alone for pure Mg and most Mg alloys. The optimum
SF6 concentration is 0?1–0?2 vol.-% as an excess con-
centration of SF6 will cause severe crucible corrosion.39
However, SF6 is becoming increasingly expensive and is
also an extremely powerful greenhouse gas, with a 100-
year global warming potential, estimated at 23 900 times
that of carbon dioxide (CO2). In addition, SF6 is
chemically stable in the atmosphere and remains present
for over 3200 years.94
Lun Sin et al. Inclusions in magnesium and its alloys
Environmental concerns have thus prompted the Mg
industry to seek alternatives to SF6. Sulphur dioxide
SO2 (approximately 1?5% in air) was demonstrated
to adequately protect molten magnesium. However,
SO2 is a toxic gas causing corrosion of foundry
equipment.92 Experiments also proved that pure CO2
effectively protects molten Mg, as long as the CO2
atmosphere is not contaminated with substantial
quantities of air.92
Other potential alternatives include
HFCs,45,48,50,52,95,96 FKs,49 boron trifluoride BF397 and
solid CO2.98,99 Hydrofluorocarbons, which include
HFC-134a (1,1,1,2-tetrafluoroethane C2H2F4),48,50
52
HFC-152a (1,1-difluoroethane C2H4F2) and HFC-
125 (pentafluoroethane C2HF5),96 have global warming
potentials 8?5–170 times lower than SF6. The protec-
tion mechanism is similar to that of SF6 with the
formation of MgF2 and MgO.45,95 Boron trifluoride
(BF3) is not a greenhouse gas and is well known for its
excellent protective behaviour. However, BF3 is highly
toxic and expensive. Boron trifluoride must also be
stored as a concentrated, highly compressed gas and,
as a result, special storage conditions are required to
minimise explosion hazard. The MagShield system was
developed to enable safe distribution of BF3.
Specifically, the gas was produced in situ by the
controlled decomposition of KBF4.97 Fluorinated
ketones49 have global warming impact similar to that
of CO2. They thermally decompose on the molten Mg
surface, producing MgF2 and CO2. They have pro-
vided protection at significantly lower concentrations
than SF6. The use of CO2 ice pellets to protect
magnesium was accomplished by injecting CO2 into
the furnace chamber at high pressure by a specially
designed nozzle. The CO2 pellets precipitate at the
molten metal surface and reduce the tendency of
magnesium to evaporate. Sublimated CO2 snow also
causes the CO2 gas to expand and displace all oxygen
from the bath surface area.98,99
International Materials Reviews 2013 VOL 58 NO 7 429
Lun Sin et al. Inclusions in magnesium and its alloys
11 Effect of filtration on the size and amount of inclu-
sions in Mg–Gd–Y–Zr magnesium alloy108
For all cover gases, care should be taken to ensure
that the gases are free of moisture and a continuous
supply of fresh cover gases is optimal.
Filtration of inclusions
One simple method to reduce the presence of inclusions
in castings is to reduce metal turbulence during melt
handling.14,100 High melt turbulence increases the
probability of entraining gases or oxide films during
mould filling, introducing more inclusions into the
casting. Incorporating filters into the casting process
helps reduce melt turbulence by regulating metal flow.
Filters must be inert, rigid, thermally stable and
thermally shockproof.101 Ideally, the filter should be
placed in the gating system of the mould (closest
location to casting) as determined by examining the
filling of a Mg plate casting using a mould with a pyrex
glass cover at a pouring temperature of 680uC. With all
other conditions being constant, the melt velocity with
no filter was 0?18 m s21 and with a filter in the runner,
0?13 and 0?14 m s21 with a filter at the gate.102
There are three stages of melt filtration:102
(i) initial surge: metal enters the filter pores and
brings the filter temperature up to the melt
temperature
(ii) normal flow: the metal flow through the filter is
constant
(iii) filter blockage: the filter becomes blocked and
metal flow stops.
Ceramic foam filters (CFFs)
CFFs consist of several open cells arranged in foam-like
structures. Ceramic foam filters are typically used to
lower inclusion levels in liquid aluminium alloys and
steels. In contrast, the performance of CFFs for Mg
alloy melts has not been studied extensively.
Bakke et al.103 studied the effect of CFFs on the level
of inclusions in AZ91 alloy. The CFFs used in their
study consisted of 68?2%Al2O3, 14?6%SiO2, 15?2%ZrO2,
1?3%TiO2 and 0?7% others (K2O, CaO, HFO2, Fe2O3
and MgO). Their results indicated that the filtration
efficiency of the CFFs was very good. Griffiths and Lai54
observed that CFFs in combination with a well designed
gating system could reduce double oxide film defects
(folded MgO films).
430 International Materials Reviews 2013 VOL 58
However, it was reported that CFFs have limited and
controversial efficiency:
(i) CFFs can react with Mg melt and contaminate
the melt.104,105 Wu et al.105 studied the potential
reactions between various CFF materials (MgO,
Al2O3, ZrO2 and SiC) and AZ91 melt during
filtration. The authors observed that molten Mg
reacted with SiC filters to form Mg2Si phases.
Under the solidification conditions studied,
Mg2Si phases exhibited a Chinese script mor-
phology, which could reduce the mechanical
properties of the alloy. The formation of Mg2Si
was confirmed by thermodynamic calculations,
which also revealed that Mg melt would react
with Al2O3 and ZrO2 but not MgO. In conclu-
sion, only MgO CFFs were suitable for filtration
purification of Mg melts
(ii) the CFFs’ adsorption ability for inclusions can
be very poor. For example, thermodynamic
calculations showed that Al2O3 filters cannot
adsorb flux inclusions in the melt. This makes it
difficult to eliminate inclusions with diameters
below 20 mm and liquid flux inclusions. In
contrast, MgO proved to have good adsorption
ability105
(iii) there is no means to determine the point where a
filter becomes ineffective and needs replacement.104
Stainless steel mesh filters
Stainless steel meshes are typically used for the filtration
of Mg melts due to their relatively low cost, high
availability and non-reactivity with Mg melts. Le et al.106
used stainless steel filters of decreased pore size in
AZ91z2 wt-%Ca alloy. They found that the finest mesh
caused a reduction in the number and maximum size of
the inclusions. Also, they determined that low pouring
temperatures (y700uC) reduced the oxidation potential
of the melt and the inclusion levels.106 Tardif et al.107
also examined the use of knitted steel mesh filters to
remove melt inclusions in permanent moulds. Two and
four ply filter configurations were examined and were
found to entrap mainly MgO and some Al–Mn–Fe
intermetallic particles.
Wang et al.108 also showed that using stainless steel
filters was an effective method to purify Mg–Gd–Y–Zr
magnesium melts. The results indicated that the average
size and volume fraction of the inclusions were
significantly reduced (56% for the average size and
76% for the volume fraction), as shown in Fig. 11.
Wang et al.109 studied the effect of stainless steel mesh
filters with various pore sizes on the melt cleanliness of
AZ31 magnesium alloy. They observed that the use of
filters proved to be an effective way to reduce the
amount of inclusions in the alloy. The average size of the
inclusions decreased from 16?5 to 2?0 mm.
Contradictory results were obtained by Emadi et al.110
In their study, the use of steel mesh filters did not lead to
a reduction in the amount of inclusions in AZ91D
permanent mould casting, with consequent absence of
improvement in mechanical properties.
Inert gas bubbling (sparging)
The refining method of gas sparging utilises an inert gas
to float melt inclusions to the surface of the melt where
they could be skimmed away. Typical gases used are
argon (Ar) or carbon dioxide (CO2). The efficiency of
NO 7

gas bubbling to remove inclusions depends on bubbling
time, gas flowrate, bubble size and melt temperature.111
Typical usage of Ar gas sparging was a flowrate of
1?8 L min21 at a melt temperature of 740uC for a
bubbling time of 30 min.111 With increasing bubbling
time and/or flowrate, the rate of inclusion removal and
hence, mechanical properties improved. Excess gas
bubbling resulted in additional porosity in the melt that
reduced strength and elongation. Argon bubbling was
effective in removing inclusions less than 80 mm, but was
unable to remove inclusions larger than 800 mm in size.41
The limited availability of quantitative results on the
efficiency of gas bubbling has sparked the need to
determine the optimal processing variables (e.g., argon
flowrate, residence time, bubble diameter, melt tempera-
ture) to enable efficient melt refining.
A combination of Ar gas sparging at 708 L h21 and a
stainless steel filter with openings of 1?14 mm (smaller
openings were more prone to plugging and choking of
metal) on recycled AZ91D Mg alloy filter has been
shown to reduce the number of non-metallic inclusions/
cm2 from 124 to 65 for the unfiltered and the filtered and
bubbled melts respectively.41 A similar result was
observed with the simultaneous use of a 20 pores per
inch (ppi) Al2O3 based ceramic foam filter and Ar
bubbling by Wu et al.112. Argon was bubbled into the
molten Mg using a rotary impeller and the optimum
bubbling conditions were determined to be 2 L h21
flowrate for 30 min at a melt temperature of 740uC.
Degassing
Melt degassing utilises typically reactive chlorine (Cl2)
gas or hexachloroethane (C2Cl6) to reduce hydrogen gas
content within melts. The addition of C2Cl6 has the
added advantage of grain refining melts, but causes
environmental problems due to the emission of chlori-
nated hydrocarbons.113 Both methods benefit from the
formation of MgCl2 (common flux component), which
can remove inclusions as discussed previously, but may
become an inclusion itself if it becomes entrapped within
the melt during pouring. Typical usage of Cl2 gas
bubbling involves heating the melt to 735–750uC and
bubbling for 5–15 min.12
Melt sedimentation (settling)
Various high density (4–7 g cm23) Fe, Si and P based
intermetallics can be removed from Mg by allowing
them sufficient time to settle in the melt.35 The required
settling time depends on the size of the crucible,
intermetallic particles and the type of holding furnace
being utilised.
Ultrasonic purification
Ultrasound can be used to treat Mg alloy melt with the
aim to enhance and accelerate the separation of
inclusions from the melt. During ultrasonic treatment
based on acoustic radiation forces, a force is exerted on
the inclusions to promote their agglomeration and
settling. Shao et al.114 found that when ultrasound was
applied, the inclusion fraction at the top layer decreased
sharply from 80?6% to 3?3%, while it increases from
16?5% to 86?6% at the bottom layer. The result indicated
that most of the inclusions suspended in the melt would
ultimately sink into the bottom layer with the help of
ultrasonic agglomeration.114 The use of ultrasound to
reduce melt inclusions is still in its infancy, but
Lun Sin et al. Inclusions in magnesium and its alloys
preliminary studies show much promise. Shao et al.115
also examined the effect of ultrasonic power andparticle
size on the efficiency of ultrasonic separation of
inclusions. Their results revealed that there is anopti-
mum ultrasonic power above which no further improve-
ment was observed. Also, at a given ultrasonic power,
smaller particles take more time to agglomerate.
If the ultrasonic treatment is based on the formation
of cavitation bubbles, high energy ultrasonic waves
disintegrate large inclusion particles into finer, less
detrimental particles more homogeneously dispersed in
the Mg melts.116
Electromagnetic separation
Electronic separation implies flotation of non-conduct-
ing inclusions in molten metal by electromagnetic force
and their subsequent removal. This technique has been
considered as a new technique to produce Mg melts free
from inclusions.117,118 Numerical simulations of steady
state laminar flow of Mg in a vertical rectangular channel
have shown that inclusion removal efficiency increases as
current density increases and channel size decreases.
However, the separation ability of the field diminishes as
the velocity of the melt increases and further research is
required to optimise the process.117,118
Alloying additions
When Mg is melted in air, the oxide film that forms by
reaction with the air is porous and unable to prevent
catastrophic oxidation. Calcium and beryllium improve
the protective quality of the reaction film,39,119 or
increase the ignition temperature of the alloy Mg.
Additions of CaO have resulted in a significant
improvement in the oxidation and ignition resistance
of Mg melts to the point where no protective gas was
required during casting.120,121 Although no melt cleanli-
ness analysis was conducted, it is expected that a
reduction of the oxidation potential could result in
lower inclusion content in the melt.
Effect of inclusions on properties of
magnesium alloys
There has been a lack of data on the effects of non-
metallic inclusions on die cast Mg.122 In this section, the
data available are reviewed.
Tensile and fatigue properties
It is known that inclusions lead to premature failure of
the material by reducing the effective cross-section of
metal under load and by the concentration of stresses at
the inclusion.
The direct impact of inclusions on the mechanical
properties is, however, difficult to quantify, since casting
defects such as cold shuts, hot tears and porosity will
normally be present alongside inclusions and dominate
over inclusions in determining the properties of a cast
part.28
This is illustrated in the work of Chen et al.116 and
Yim et al.111 Chen et al.116 studied the effect of
ultrasonic treatment on the microstructural and
mechanical properties of AZ91 and AM60 alloys. It
was found that the application of ultrasound to the melt
led to the fragmentation of oxide films. Inclusion
particles became smaller, more numerous and better
distributed in the melt. Smaller inclusion particles were
International Materials Reviews 2013 VOL 58 NO 7 431
Lun Sin et al. Inclusions in magnesium and its alloys
12 Effect of metal cleanliness on the mechanical proper-
ties of die cast AM5028
preferable to the larger ones and should result in
improved mechanical properties. However, gas pores
and air pockets were also entrapped in the alloys during
solidification, leading to a reduction of the UTS and the
elongation.
Similarly, gas bubbling led to the removal of
inclusions in AZ91D melt.111 This was, however,
accompanied by the formation of pores in the casting.
Consequently, the tensile elongation of the alloy was
found to decrease.
For defect free castings (hot tears, porosity, folds,
etc.), the inclusion content and distribution of inclusions
are assumed to be a critical factor in determining
mechanical properties.28 A significant improvement in
the tensile properties (ultimate tensile strength and
elongation)30,41,62,81–84,86,102,107,108,122 and the impact
strength62,122 with the reduction of inclusion content in
the melt was indeed observed by several researchers.
The stress–strain curves (Fig. 12) for AM50 alloy
containing different levels of inclusions suggest that
castings made using clean melts fracture at significantly
higher strain than castings made using contaminated
melts.28 An inclusion level of 500 ppm was found to be
the highest acceptable inclusion content.
Mirak et al.53 showed that improving the running
system design can lead to increased ultimate bend
strength from 180 to 400 MPa, as a result of the
reduction of the in-gate velocity from 1 to 0?25 m s21.
The Weibull modulus also increased with a reduction of
the in-gate velocity, indicating decreased scatter of
mechanical properties and improved reliability of the
castings. This was attributed to a reduction of surface
turbulence and double oxide films in the castings.
Elsayed et al.124 observed that steel mesh filters with
wire diameters of 0?4 mm and mesh size of 0?860?8 mm
increased the mechanical properties of permanent mould
cast AZ91E. Without a filter, the AZ91E alloy had an
average yield strength, tensile strength and elongation of
93 MPa, 155 MPa and 2?26% respectively, which
increased to 97 MPa, 167 MPa and 3?18% respectively
with the use of a filter. The improved mechanical
Table 7 Effect of filtration and gas bubbling on UTS and elongation of AZ9194,101
Refining treatment
No treatment
Filtration (ceramic foam filter, 20 ppi, 20 mm thick)
Argon bubbling (flowrate: 2 L min21, bubbling time: 30 min)
Argon bubblingzfiltration
432 International Materials Reviews 2013 VOL 58
properties were attributed to the removal of oxide
inclusions and the reduction of turbulence during
casting.
Wang et al.109 observed that the tensile properties of
AZ31 alloy improved with the use of stainless steel mesh
filters. The ultimate tensile strength and elongation of
the alloy increased from 194 MPa and 13?8% to
212 MPa and 20?3% respectively.
Similarly, Tardif et al.107 showed that melt filtration
of AZ91 alloy produced consistently sound castings with
improved tensile properties. Nazari et al.102 and
Griffiths and Lai54 also showed that filtered castings
exhibited higher Weibull moduli than unfiltered cast-
ings, indicating that the mechanical properties of the
alloy were more consistent and reproducible.
Wu et al.105,112 investigated the effect of filtration and
gas bubbling on the ultimate tensile strength and
elongation of AZ91. There was significant improvement
in the UTS (10%) and the elongation (6%) with argon
gas bubbling and filtration (Table 7).
Haerle et al.62 obtained similar results. There was a
further improvement of the mechanical properties when
gas bubbling was combined with melt filtration, in
agreement with Housh and Petrovich.41
In regard to C2Cl6 addition, Emadi et al.110 showed
that without any pretreatment, the as cast yield strength,
tensile strength and elongation of AZ91D alloy were
78 MPa, 176 MPa and 4?4% respectively. With the
addition of 0?3 wt-%C2Cl6, the grain size decreased from
88 to 56 mm and the castings showed much fewer and
smaller inclusions on the fracture surface. The yield
strength, tensile strength and elongation increased to
92 MPa, 200 MPa and 5?1% respectively. In the case of
AZ31 alloy, the yield strength, tensile strength and
elongation were 52?0 MPa, 161?0 MPa and 14?5%
respectively. When 0?2 wt-%CaO was added to AZ31,
these properties increased to 74?9 MPa, 175?9 MPa and
18?0% respectively.120 In both cases, the improvement in
mechanical properties was attributed to both grain
refinement and inclusion removal.
The addition of a C2Cl6–KCl mixture was also
found to improve melt cleanliness of recycled AZ91E
castings.124 Upon remelting twice, the casting elongation
reduced from 3?18% to 2?15% as compared to the virgin
casting. The melt was cleaned of oxides with the
addition of 1?0 wt-% C2Cl6–KCl mixture resulting in
an improvement in mechanical properties and elonga-
tion. The casting after remelting twice had a tensile
strength and elongation of 171 MPa and 2?15% respec-
tively and increased to 195 MPa and 4?03% respectively
with the addition of the C2Cl6–KCl mixture.
Researchers from Shanghai Jiaotong University per-
formed several studies on GW103K (Mg–10Gd–3Y)
type alloy.81–84,86,108 They investigated the separate and
combined effect of filters and various fluxes on the
mechanical properties of GW103K. The use of fluxes
resulted in the removal of inclusions in the melt, which
UTS/MPa Elongation/%
175.3 2.74
189.1 4.02
180.6 3.53
192.1 4.22
NO 7

in turn led to a significant increase in the ultimate tensile
strength and elongation. Wang et al.82 also studied the
effect of MgO ceramic foam filters on the properties of
GW103K. As compared to the untreated samples, the
mechanical properties were higher but remained inferior
to those obtained by using a flux, as the filter only
removed large inclusions. In another study on Mg–Gd–
Y–Zr alloy, the YS, ultimate tensile strength and
elongation were improved from 156 MPa, 200 MPa
and 3?4% to 167 MPa, 232 MPa and 7?0% respectively
with the use of filters.108 A similar study was performed
on AZ91 alloy.30 Again, it was found that the use of flux
improved the mechanical properties of the alloy. The
mechanical properties were further enhanced by com-
bining the use of flux with ceramic foam filtration.
It should be noted that small oxide inclusions play a
minor role in influencing tensile properties of castings.
In a study by Wang et al.,123 the results indicate that
oxide contents up to 1000 ppm levels have apparently
no effect on tensile properties when most oxides are
less than 15 mm and oxide films are less than 50 mm in
size.
It is also accepted that fatigue life decreases sig-
nificantly with inclusions size. In AZ91E alloys,
Horstemeyer et al.125 have shown that if the inclusion
size is reduced from several millimetres to several
hundred microns, the fatigue life in the high cycle fatigue
regime can be increased by two orders of magnitude.
Fluidity
Inclusions can increase the viscosity of the melt, thereby
impairing its fluidity. Also, if oxides are present, they
have a tendency to form as films and these can block
feeding channels and result in incomplete filling.126
Bakke et al.28 found that the flow length (measured
using a meander die) of AM50 alloy was decreased by
10–20% in a contaminated melt. The reduction of
inclusion content in the melt leads to an increase in
the fluidity, as illustrated in Table 8.58 Similar results
were obtained by Wang et al.82 and Wu et al.127
Corrosion resistance
Inclusions have a deleterious effect on the corrosion
resistance of Mg alloys.82–84,108,122,128 As an example,
Wang et al.82 studied the effect of inclusions on the
corrosion rate of Mg–10Gd–3Y–0?5Zr alloy. They
Table 8 Effect of MgO content on average fluidity length
of AZ91 alloy measured using spiral shaped
permanent mould58
AZ91 alloy MgO content/ppm Average fluidity length/mm
1 35¡6 225
2 42¡12 220
3 75¡19 203
4 93¡24 192
5 125¡64 185
6 472¡345 172
Table 9 Effect of inclusion content on corrosion rate of Mg–10Gd–3Y–0?5Zr alloy82
Average volume fraction of inclusions/%
4.07
2.84
0.87
Lun Sin et al. Inclusions in magnesium and its alloys
observed that the corrosion rate increased with increas-
ing average volume fraction of inclusions, as shown in
Table 9. This was attributed to the difference of
electronegativity between the inclusions and Mg matrix.
The inclusions act as cathodes and form galvanic
coupling with the matrix, leading to pitting corrosion.
With increasing inclusion content, the cathodic area
increases, thereby adversely affecting the corrosion
resistance of the alloy.128
Machinability
Haerle et al.122 studied the effect of non-metallic
inclusions on the machinability of AZ91D alloy. They
observed that a larger volume of inclusions contributed
to a greater degree of wear of the cutting tools. As a
result, the force required to cut AZ91D increased. The
machinability of AZ91D was thus reduced.
Conclusions and perspectives
Types of inclusions and their control
Limited information on refining of Mg alloys is
available, as compared to Al alloys. Inclusions present
in molten Mg can be categorised into two major groups:
non-metallic inclusions (mainly oxides and chlorides)
and intermetallic inclusions (iron rich phases). These
inclusions arise from various sources, which include the
charge (quality of metals and alloys), melting process,
reaction with fluxes and protective gases (during
melting, transfer and pouring processes) and reactions
in the mould. Several methods are available to control
inclusions in Mg alloys.
(i) fluxes, consisting of MgCl2 and other chlorides
(e.g. KCl, NaCl), protect Mg melts from oxida-
tion. However, typical fluxes used for the
refining of Mg alloys are not compatible with
all alloys, such as those containing calcium,
strontium and rare earth elements.
(ii) fluxless methods include use of protective gases,
filtration, gas bubbling and electromagnetic
separation
(iii) addition of some alloying elements (e.g. calcium
or beryllium) to Mg melts reduces the oxidation
potential of Mg and consequently the inclusion
content in the melt.
Melt cleanliness
Assessment of Mg melt cleanliness can be performed
through physical measurement methods (FNAA, GD-
MS and GD-AES). Though highly sensitive and
accurate, these methods remain very expensive.
Recently, techniques such as fracture surface examina-
tion, filtration of liquid metal and subsequent analysis of
inclusions filtered, wet chemistry method, self-gravita-
tion filtering technique and ultrasonic analyser have also
been considered. However, there is no widely accepted
criterion for testing Mg melt cleanliness.
Corrosion rate/mg cm22/day
2.0
1.8
1.3
International Materials Reviews 2013 VOL 58 NO 7 433
Lun Sin et al. Inclusions in magnesium and its alloys
Inclusions and properties
The use of filters, inert gas bubbling, fluxes and degasser
addition are all effective methods to improve melt
cleanliness and mechanical properties of Mg alloys.
Improvements of 15% in tensile strength and 100% in
elongation are possible. Combination of filtration and
other techniques could further improve melt cleanliness
and mechanical properties.
The presence of inclusions can also reduce melt
fluidity and corrosion resistance of castings. The
presence of inclusions will increase viscosity of melts
making them more difficult to cast and form galvanic
coupling with the matrix, leading to pitting corrosion.
The presence of non-metallic inclusions will also
prematurely wear cutting tools and as a result, reduce
the machinability of Mg alloys.
There is a need to understand and control all aspects
of metal handling and processing to improve quality and
consistency of the cast product.
Perspectives
Assessment of melt cleanliness
None of the techniques developed to assess the melt
cleanliness of Mg alloys has been universally accepted.
Metallographic techniques, humidity tests and K-mould
fracture samples have been invaluable tools used in the
foundry shop, but there is still a need for an efficient and
economical assessment technique. A combination of
methods may be needed. Future areas of research should
aim at utilising filtration methods such as self-gravita-
tion and HMIAM as these techniques are relatively
easier to implement on a foundry scale and are of
relatively low cost.
Control of inclusions
The methods used to control the inclusions in the melt
need to be optimised, since some results are contra-
dictory and quantitative results are missing. Most
importantly, the process costs to achieve acceptable
quality are sometimes prohibitive.
Understanding of inclusion formation and influence on Mg
alloy properties
The majority of inclusion related issues with Mg alloys
appear to originate with the molten Mg being exposed to
moisture or oxygen. This is an issue during melting, melt
transfer before pouring and mould filling. There is a
need to determine the Mg melt quality at all stages of the
casting process. Better understanding of the behaviour
of oxide films (in particular bifilms) within the molten
metal would help determine the best foundry practices to
reduce their formation and entrapment in Mg melts.
Acknowledgements
The authors are indebted to Professor A. McLean for
his review and valuable comments. They thank the
members of the Centre for Near-Net-Shape Processing
of Materials, in particular A. Machin, J. Hill, S. Ahmad
and E. Vandersluis for their suggestions. They sincerely
acknowledge the Natural Sciences and Engineering
Research Council of Canada for financial support.
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