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H. W. Doty
Materials Engineering, General Motors, Pontiac, MI, USA
Abstract
The present investigations were carried out on experi- recommended that the Brightimeter readings (indices)
mentally prepared AM50A and AZ91D alloys. The main should be coupled with metallographic examination. The
thrust was the application of the Brightimeter technique in main inclusions are magnesium oxides (MgO), magnesium
quantifying the concentration of the inclusions in these hydroxides (Mg(OH)x), aluminum oxides (Al2O3), spinel (a
alloys. The results show that the Brightimeter indices are mixture of MgO ? Al2O3). In some cases, pure metals such
low when the amount of oxides, i.e., MgO, Al2O3, Al2MgO4 as iron (Fe) and aluminum (Al) were also observed along
is high. Reducing the oxide concentration increases the with their oxides, i.e., FeO and Fe2O3. The use of flux as a
Brightimeter readings (indices). It is concluded that the protective agent may cause the presence of other types of
Brightimeter apparatus is an effective technique in deter- inclusions such as K, Na and Ca. The quantity of oxides
mining the metal cleanliness in terms of detecting and depends to a large extent on the inclusions initially present
measuring the inclusion content. Its sensitivity increases in the as-received alloy. Recycled alloys were found to
with the increase in the amount of inclusions. At low levels contain the maximum amount of inclusions.
of inclusion concentration, there is a noticeable fluctuation
in readings of the Brightimeter. The main parameter to be Keywords: magnesium alloys, inclusion measurements,
considered is the melting and solidification process. It is Brightimeter technique, metallography, microstructure
Table 1. Chemical Composition of the Experimental Mg– smaller Fe-based intermetallic inclusions. Whereas ZE41A
Al–Zn Alloys Used in the Present Study alloy was susceptible to many small inclusions, AZ91D
Alloy code Mg% Al% Zn% Mn% alloy was more susceptible to few large inclusions. The
film-type inclusions for ZE41A would tend not to
AM50A 95.56 4.00 0.44 0.13 agglomerate and are reasoned to be not as harmful as the
AZ91D 90.00 9.00 1.00 0.26 agglomerated and faceted particle-type inclusions with
large surface area observed in the AZ91D alloy.
manpower. Elsayed et al.5 studied inclusions in permanent Haerle6 proposed a simple technique to measure and
mold cast magnesium ZE41A and AZ91D alloys. Their quantify the amount of inclusions in Mg-based alloys. The
results show that the fracture surfaces of the ZE41A alloy principal idea of this technique is that the incident light on
contained film-type Mg–O-based inclusions, whose poor any metallic surface is reflected, absorbed or diffracted by
interface with the matrix was likely the source of fracture. the surface of the metallic object. The instrument used by
The AZ91D alloy fracture surfaces contained mostly par- Haerle is registered under the commercial name Techni-
ticle-type Mg–Al–O spinel inclusions, as well as few dyne BrightimeterTM, model A4M. Figure 1a is a
Experimental Procedure
Figure 4. (a) Distribution of the Brightimeter readings in 100% fresh alloy. (b) Distribution of the Brightimeter
readings in 100% recycled alloy.
Figure 5. (a) Distribution of the Brightimeter indices in 100% fresh AZ91D alloy. (b) Distribution of the
Brightimeter indices in 100% recycled AZ91D alloy. Arrows indicate the possibility of large chunks of oxides.
Figure 6. Percentage of inclusions-Brightimeter index relationship in: (a) AM50A alloy, (b) AZ91D alloy.
25
Dirty
25 fields 100 fields 200 field
20
% Inclusions
15
10
5
Clean
0
1 2 3 4 5 6 7 8 9 10 11 12 13
Sample #
Figure 9. Backscattered electron images of: (a) AM50A alloy and (b) AZ91D alloy.
Brightimeter index
50
Brightimeter index
110 50
110
48 48
100 100
46 46
90 90
44 44
80 80
42 42
70 40 70 40
60 38 60 38
50 36 50 36
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Samples # Samples #
Figure 10. Average grain-size-Brightimeter index relationships in: (a) AM50A alloy and (b) AZ91D
alloy. Note #1 is grain size, and #2 is Brightimeter Index.
Figure 11. Optical micrographs showing examples of the types of oxide films
observed in the AM50A alloy: (a) snaky type oxides, (b) long oxides and AZ91D
alloy, (c, d) mixtures of porosity (arrowed a) and oxide films (arrowed b).
the corresponding Brightimeter readings. In the case of the AZ91D alloy, Figure 6b, the relation between the results
AM50A alloy, the percentage of inclusions obtained for the from the two methods of measurements is linear rather than
various samples examined is spread over a wide range. parabolic. However, it should be noted that for both
Two mathematical correlations were applied, linear and regression methods, the fitting coefficient is \0.8.
parabolic. It is clear from Figure 6a that the relationship
between the two methods is parabolic rather than linear, Another parameter to be considered in using the image
due to the presence of large amounts of oxide films of analyzer system is the number of measured fields. In the
different sizes caused by the increase in the aluminum case of highly contaminated (dirty) alloys, an examination
content. These results are in good agreement with the of at least 200 fields at 1009 are required to obtain a
findings reported by Grebetz et al.10,11 Considering the reliable value, which may not be necessary in the case of
O 32.3 60.7 Figure 10 illustrates the effect of the grain size on the
Brightimeter readings. As may be seen, the grain size has
K 6.7 5.1
no specific role in controlling the Brightimeter index value.
Mn 6.4 3.5
In the event that the grain size is large—which may affect
Ti 25.9 16.3 the reflecting light beam, with rotation of the sample every
Fe 25.5 13.8 36 degrees, this effect becomes negligible.
Total 97.4 100.0
Types of Inclusions
clean metal. In the present study, all reported values were Optical Microscopy
obtained by examining 200 fields in each case/sample.
Figure 7 shows how the percentage of inclusions observed In order to arrive at a better understanding of the rela-
in a particular sample can vary, depending on the number tionship between the amount of inclusions and the corre-
of fields measured. sponding Brightimeter indices, metallographic samples
were prepared from both ‘‘clean’’ and ‘‘dirty’’ samples.
One of the main concerns in the use of the Brightimeter Figure 11a and 11b shows examples of the oxide films
technique is the role of the alloy composition on the surface observed in the two alloys termed ‘‘clean’’—Brightimeter
brightness of the alloy sample. The variation in the Al and Zn indices around 52–58. Figure 11c and 11d reveals a mix-
content changes the gray level of the Mg–Zn–Al phase and ture of porosity and massive oxide films in samples termed
hence the Brightimeter index for the level of inclusions. This ‘‘dirty’’—Brightimeter indices around 32–35.
observation is well illustrated in Figure 8 which shows the
Brightimeter index values for 100 samples covering 5 levels
Electron Probe Microanalyzer
of Al content. It is evident from this figure that most of the
points are segregated around an index value of 55—see
AM50A Alloy
circled area. At a low level of aluminum, the fractured sur-
face is bright, resulting in the high index values observed. As
for alloys containing 14% Al, the fractured surface is rather All electron micrographs presented in this section were
gray which is reflected in the corresponding Brightimeter taken from ‘‘dross’’ samples with Brightimeter indices in
readings. Figure 9 shows the size and distribution of the Mg– the range of 27–35. During the fabrication process of pure
Zn–Al phase particles observed in the AM50A and AZ91D Mg, certain amounts of salt may be trapped in the liquid
alloys. Since the AM50A alloy has less Al content and metal and remains after solidification. Figure 12 shows an
Figure 13. EDS spectrum corresponding to the backscattered image in Figure 12a.
Table 3. WDS Analysis of Phase Marked 1 (a), Marked 2 oxides. Taking into consideration that the crucible used for
(b), Marked 3 (c) in Figure 14 melting is made of mild steel, thus a piece of Fe may have
fallen in the liquid metal prior to pouring in the metallic
AM50A wt% at.% mold.Figure 13 shows the EDS spectrum corresponding to
(a) the backscattered image in Figure 12a. Figure 14 illustrates
an example of Fe-based oxides observed in the
O 24.3 53.2
generic AM50A alloy. The WDS analysis listed in
Fe 73.9 46.4 Table 3a–c identifies these oxides as FeO, Fe2O3 and Fe,
Total 98.6 100.0 respectively.
(b)
O 25.2 57.6 Magnesium has a higher affinity to react with oxygen than
Fe 60.8 39.8 aluminum as shown in Figure 15.15 Figure 16 is a good
Total 88.2 100.0
example illustrating this statement. Table 4a shows the
chemical analysis of area marked A. The WDS analysis of
(c)
area ‘‘B’’ in Figure 16 is shown in Table 4b which is
O 0.7 2.4 mainly MgO-Al2O3 (spinel). The absence of Al in area
Fe 98.3 97.0 ‘‘C’’ in Figure 16 indicates that the composition of this
Total 99.3 100.0 phase is only MgO. The associated WDS analysis pre-
sented in Table 4c reveals that the total weight percentage
of the elements in this phase is less than 100%. Thus, it
example of a salt particle observed in the experimental may be reasonable to assume that the chemical composi-
AM50A alloy, whereas Table 2 lists its chemical compo- tion of this phase is rather Mg(OH).
sition revealing a mixture of oxides, including Fe-based
Figure 17 displays a mixture of oxides in the AM50A long. It should be mentioned here that no vigorous
alloy. The backscattered image is divided into four areas mechanical stirring was applied at any stage of the work.
according to their gray level. The presence of Mg and O Also, the molten metal was kept under dynamic protective
only indicates that areas A and D are MgO. The black area gas during the melting and solidification processes.
marked ‘‘B’’ is a pore as evidenced from the absence of any
element, whereas the matrix (marked C) is mainly Mg. Figure 21 reveals the presence of a massive ‘‘chunk’’ of
Figure 18 displays the presence of a shrinkage network. oxides in the dross. The colored map shows that the area
The colored map reveals high oxygen and magnesium marked ‘‘A’’ contains Al, Mg and O2 which indicates that it
intensities within these cavities. Also, their surfaces are is spinel (Al2MgO4).16 Area B contains only Mg and O2
rough compared to the surrounding Mg matrix. giving rise to the formation of MgO. Area marked ‘‘C’’
contains Ca, O2 and Al makes it possibly CaOAl2O3.
Figure 22 shows the presence of some amount of Ca
AZ91D Alloy compounds. Since Ca was never introduced during the
melting process, thus the only source is the flux used for the
Figure 19 demonstrates the distribution of the elements in a production of the Mg used in the study. Calcium by itself
group of MgO bi-films observed in the experimental AZ91D may be from the primary magnesium production method.
alloy. Both Al and Zn show more or less similar intensity. KCl, on the other hand, is from flux contamination (i.e.,
Figure 20 shows that MgO can as well precipitate in the form improper settling prior to transfer from the refining process
of bulky or massive areas almost 200 lm wide and 1000 lm to the casting process).
Table 4. WDS Analysis of Areas Marked ‘‘A’’, ‘‘B’’ and ‘‘C’’ Summary
in Figure 16
The fluctuation in the Brightimeter index values is low
AM50A wt% at.% when highly contaminated samples are used. With the
(a)
increase in the sample level of cleanliness, the scatter in the
Brightimeter readings is relatively high. All alloys behave
O 2.5 4.7
in the same manner and may be divided into two cate-
Mg 1.7 1.8 gories, corresponding to clean and dirty melts. The
Al 96.6 93.5 microstructure and hence the gray level of the reflecting
Total 101.7 100 sample surface is an important parameter to consider when
(b) using the Brightimeter technique. Thus, a metallographic
O 19.9 27.4 study should be carried out simultaneously to support the
former. The Brightimeter technique is insensitive to the
Mg 67.7 61.3
presence of porosity when the latter is mixed with oxide
Al 12.4 10.1
films. Grain size, as such, has no specific bearing on the
Total 102.0 100.0 Brightimeter readings.
(c)
O 59.0 70.7 The principal inclusions existing in fresh (i.e., un-recycled)
Mg 36.9 29.1 alloys are MgO and Mg(OH), Al2O3 or a regrouping of
Total 96.3 100.0 oxides such as Al2O3MgO. In some cases, metal oxides
(FeO, Fe2O3) may form from either the steel crucible or