Construction and Building Materials 90 (2015) 68–79

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Construction and Building Materials

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Electric arc furnace slag and its use in hydraulic concrete

Idoia Arribas a, Amaia Santamaría b,⇑, Estela Ruiz c, Vanesa Ortega-López d, Juan M. Manso d
a
TECNALIA, c/Geldo – Parque Tecnológico de Bizkaia, Edificio 700 48160 Derio, Spain
b
Mining, Metallurgical and Materials Science Department, University of Basque Country, Alameda de Urquijo s/n, 48013 Bilbao, Spain
c
LADICIM E.T.S. Ingenieros de Caminos, Canales y Puertos, University of Cantabria, Av/Los Castros s/n, 39005 Santander, Spain
d
Civil Engineering Department, EPS University of Burgos, Calle Villadiego s/n, 09001 Burgos, Spain

h i g h l i g h t s

 EAF slag is a rocky material of use in construction and civil engineering.

 EAF slag shows some chemical changes and slight expansiveness over time.
 Collaboration producers-consumers of EAF slag is essential to efficient re-use.
 EAF slag is a suitable aggregate for hydraulic cement concrete.
 EAF slag forms a particular type of microstructure in the interfacial transition zone.

a r t i c l e i n f o a b s t r a c t

Article history: Electric arc furnace oxidizing slag (EAFS) is a by-product of the steelmaking industry, generated after the
Received 15 January 2015 melting and the preliminary acid refining of liquid steel. It is a stony material that is easy to crush for use
Received in revised form 16 March 2015 as aggregate in concrete mixes.
Accepted 1 May 2015
This study examines the long-term aging reactions of EAFS and its volumetric stability, to gain further
Available online 16 May 2015
knowledge of this by-product, its behaviour as a construction material, and its inherent risk of swelling.
Additionally, the good compressive strength of hydraulic mixes that incorporate this slag can be analyzed
Keywords:
and explained on the basis of its steady and expansive compounds and its chemical evolution over time in
Electric arc furnace oxidizing slag
Expansive compounds
the interfacial transition zone (ITZ); the appearance of calcium carbonate enhances the cohesiveness,
Slag weathering stiffness and strength of this zone and, as a consequence, of the hydraulic concrete.
Accelerated aging Ó 2015 Elsevier Ltd. All rights reserved.
Recycled aggregate
Hydraulic concrete
Interfacial transition zone
ITZ

1. Introduction techniques for their reuse [4–20]. Several investigations on the

re-use of steelmaking slags have been published over the last dec-
The sustainability of human activity has become a key issue in ades; some of them concerning mortar and concrete (rigid-stiff
the last decade of the 20th century and the first decade of the 21st matrices) [21–43], and mixtures with granular soils
century. The search for sustainability has driven the reuse of suit- (compliant-flexible and porous matrices) [44–58].
able industrial by-products with the right properties, thereby Electric arc furnace oxidizing slag (EAFS) is a by-product of the
reducing the consumption of natural resources. Since the pioneer- steelmaking industry, generated after the melting and the primary
ing papers of Motz, Geiseler and Koros [1–3], almost all kinds of acid refining of liquid steel. Its chemical composition is based on its
iron and steelmaking (as well as other metal) slags have been pro- content of calcium, iron and silicon oxides in a global amount of
posed for use in construction and civil engineering. Researchers over 80%; aluminium, magnesium, manganese and phosphorus
now face the task of finding the most efficient and appropriate oxides are also present. Variations in the proportion of these oxides
are due to the kind of steel, the refractory materials of the furnace
⇑ Corresponding author at: Engineering School of Bilbao, University of the Basque and some technological advances. In standard oxidizing electric arc
Country, 48013 Bilbao, Spain. Tel.: +34 34 601 7319. furnace slag (EAFS), the proportion of acid oxides (silica, alumina,
E-mail addresses: [email protected] (I. Arribas), amaia.santamaria@ iron oxide . . .) is predominant on the proportion of basic oxides
ehu.es (A. Santamaría), [email protected] (E. Ruiz), [email protected] (lime, magnesia and alkalis).
(V. Ortega-López), [email protected] (J.M. Manso).

http://dx.doi.org/10.1016/j.conbuildmat.2015.05.003
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79 69

The similarity between the oxides, which may even be present in its application, which require a wide range of scientific analyses
in similar proportions in both EAFS and LD converter slag [76,77]. The immediate effects of the addition of large amounts of
(Linz-Donawitz converter slag) or BOF-slag, (Basic Oxygen EAFS aggregate (on fresh and hard concrete) are loss of workability
Furnace slag) and their common stony-gravel presentation, might and an increase in the short-term mechanical properties (strength
lead to the erroneous impression that they are the same material. at 7 and 28 days). These and other important questions (i.e. dura-
However, these products differ slightly, due the lower amount of bility tests) have been studied by the authors over the past decade
free calcium oxide, CaO, also called free lime [59–68] in the EAFS, and their results and opinions form part of the scientific literature.
which also explains its lower expansiveness. Nowadays, the use The main compounds of EAFS, according to the scientific litera-
of EAFS as a coarse aggregate in hydraulic concrete is widely ture, are single and complex calcium silicates (containing alu-
accepted, while LD-slag is mainly applied in roadbeds. Maximum minium or magnesium) and single and complex iron-based
levels of volumetric expansion in materials used as concrete aggre- oxides (containing calcium, magnesium, chromium, manganese,
gates and as roadbedding are set at around 1% and 5%, respectively, among others) which are in a liquid state above 1500 °C, aided
in current standards. by fluxes such as CaF2, which solidify at under 1200 °C. Silicates
Pioneering papers that detailed rigorous, systematic and global (dicalcium silicate b or c belite-larnite, ackermanite, gehlenite,
studies of the use of EAFS in mortar and concrete were published in wollastonite, calcium-olivine, kirschsteinite, melilite, and others)
Japan between 1991 and 1999 by K. Morino et al. [69–71]; other and iron-based oxides (wustite, magnetite, hematite, dicalcium
publications in the same field over the same decade were less sys- ferrite, R-O phase. . .) can be considered to add to short-term stabil-
tematic. At the start of the 21st century, their work and those of ity, although their long-term chemical stability is not evident and
other Japanese authors [72–74] were published in English, and sev- has to be verified. The undesirable presence of metallic iron in
eral new research teams begin to work on this subject. Our team the slag must be eliminated through efficient magnetic separation.
began its research in this field in 1997, beginning with the PhD Additionally, fresh EAFS slag (unweathered, after cooling) often
Thesis of Prof. Manso; an initiative now exists among several EU contains small amounts of free-CaO (also called free-lime) dis-
research groups to establish pre-normative standards in this field. persed in its microstructure. Despite its presence, some of the ana-
The present study deals with EAFS expansion following sponta- lytical procedures to quantify its amount in the slag are unreliable.
neous (weathering) and accelerated testing and, subsequently, its A more precise method of quantifying free-CaO content in EAFS is
particular application as a coarse aggregate in hydraulic concrete. accelerated aging until total hydro-carbonation is achieved, fol-
The composition and characteristics of EAFS are studied by means lowed by thermo-gravimetric heating analysis up to 900 °C.
of standard analytical techniques: X-ray diffraction, thermogravi- Several reasons explain the volumetric instability of generic
metric and differential calorimetric scanning analysis, metallurgical slags. Firstly, the evolution of silicate b to c is accom-
low-vacuum SEM microscopy and EDX analysis. This article, based panied by an increase in volume, although this reaction is less
on the PhD Thesis of Ms Idoia Arribas, extends the results and adds likely in EAFS, due to the presence of P2O5 and other b-phase sta-
subsequent findings from the research team. The long-term evolu- bilizers. Secondly, the long-term oxidation of metallic iron from
tion of EAFS is studied, especially in terms of CaO migration, which iron +2 to iron +3, although infrequent, has also been observed in
is related to the characteristics of the Interfacial Transition Zone metallurgical slags. Thirdly, it has been observed a
(ITZ) observed in the concrete mixes, leading to interesting results low-temperature hydroxylation of free-CaO and subsequent car-
and relevant conclusions. bonation, in the presence of moisture, and even of free-MgO,
although the latter is uncommon in EAFS. These reactions are asso-
ciated with a significant increase in volume, sometimes with
2. Background on EAFS short-term and at other times with long-term effects.
According to the scientific literature [61,66], the free lime found
After cooling from 1580 °C, the EAFS by-product becomes a in LD-slag can be divided into two groups. The first group is resid-
stony, cohesive, slightly porous, heavy, hard and tough material, ual free lime (not completely dissolved in a liquid state) that is
the initial colour of which is almost black, due to the presence of grainy or spongy with particle sizes of between 2 and 40 microns.
iron oxides. Long-term outdoor weathering causes its colour to The second group, precipitated free lime, is smaller than 4 lm and
change to clear-grey shades. It is easily crushed, its residual metal- may be found in the grain boundaries of some iron-oxide-based
lic iron must be mostly separated, and it can then be employed as compounds (dicalcium ferrite or R-O phase), either dispersed in
coarse and fine aggregate in hydraulic mortars and hydraulic or the calcium silicates, in SC3 crystals or in SC2 crystals. Both are
bituminous concrete. Its other possible uses include bedding mate- found in EAFS, although the latter are by far the most common.
rial for roads and railways, and water depuration, as well as soil Despite the fact that EAFS is an ‘‘oxidizing’’ slag, in which the
stabilization and correction. predominant acid oxides are capable of dissolving all of the basic
All aggregate materials to be applied in concrete have to be oxides, it is not uncommon to find some types of EAFS that contain
analysed in depth before their use can be standardized. Problems undissolved particles of free-CaO. These particles are a conse-
of alkali-aggregate reactions and intrinsic chemical instability are quence of the electric arc furnace procedure; partial addition of
examples of the risks associated with the use of certain natural lime is sometimes made near the end of the ‘‘acid’’ refining process,
minerals as aggregates. In the case of EAFS, an artificial material, without sufficient time for the other acid slag components to dis-
there is a general consensus that its chief problem is volumetric solve this lime. Finally, this free-CaO remains undissolved in the
expansiveness or swelling of pieces, lumps and particles, due to mass of the slag as it cools.
the chemical activity of expansive compounds such as free-CaO Furthermore, other operations such as the ‘‘foaming’’ of the slag
and, sometimes, free MgO-periclase, an expansive compound that in the electric arc furnace, the pouring process, and slag cooling
has scarcely been reported in the literature [75]. Their presence method to room temperature all form part of the steelmaking pro-
is detrimental and should be carefully monitored when the con- cess. There are at least two methods for cooling EAFS, from furnace
crete is prepared and throughout its in-service life. temperatures to room temperature. One method is cooling in con-
The main physical and chemical characteristics of EAFS for use tinuous mode, dousing a small flow of slag with water and obtain-
as mortar and concrete aggregate, which influence its weight and ing particles, lumps and pieces of a size under 40 mm; these
integrity, are its high density and its free calcium oxide content. particles may be used as gravel after metallic iron separation.
Further relevant characteristics have to be analysed and evaluated The other method involves pouring the liquid slag into a large pit
70 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79

in a liquid state, depositing a new layer on the last layer of solidi- dioxide react to give soluble calcium bicarbonate (CO3H)2 Ca. The
fied slag, while several water jets cool the upper surface. The cool- migration of this compound when dissolved in water to the surface
ing rate of the slag in the latter case is lower than it is in the former of the external slag pieces or particles, and the subsequent evapo-
case; thermal contraction and spontaneous shrinkage break up the ration of the water left the visible precipitation of white calcium
slag into pieces of more than 40 mm in size, followed by subse- carbonate. A fraction of the free-CaO might not be accessible to
quent crushing and metallic iron separation. The aforementioned humidity and it should be noted that some of it may remain in
operations determine very important aspects in the use of EAFS, an unreacted state, cloistered in the microstructure of the slag.
such as in-solid-state porosity, density, metallic iron content, inter- Moreover, when EAFS is used as aggregate in hydraulic mixes,
nal presence of cracks or crevices, and initial grading; these oper- there is a zone of the material, mortar or concrete, that is directly
ations define the final quality of the EAFS for re-use in the affected by the slow arrival of CaO, due to the aforementioned dif-
construction and civil engineering sectors. Steelmaking procedure fusion mechanism in the presence of humidity. This interfacial
therefore has a central influence on the quality of the EAFS that transition zone (ITZ), between the aggregate particles and the
is produced; in the past, steelmakers were not concerned with cementitious matrix, is considered a weak zone of the concrete.
the quality of their slags as most of it was dumped in landfill sites. In this region, the appearance of micro-bleeding around the aggre-
Nowadays, collaboration between the producers and the con- gate particles, porosity and some microstructural features depend
sumers of this material is essential and it would probably be an on several factors, such as aggregate quality and size, the
appropriate time to encourage such collaboration within the EU. water-cement ratio, the binder and the age of the mix. The mor-
The density (q) of EAFS has been recorded within the range of phology and properties of the ITZ evolve at the same time as the
3–4 Mg/m3. It depends mainly on the content of metallic iron hydraulic reactions of the Portland cement take place [78–82].
(q  8), iron oxides (q  5) and the internal porosity. In construc- Following the excellent and exhaustive dissertation on the ITZ
tion and civil works, a higher density than ordinary concretes is in the book of Mehta and Monteiro [83], there have been few out-
sometimes required (marine-coastal blocks, retaining walls, standing advances in the scientific literature. Several interesting
foundations or great basement slabs), but it is sometimes compul- works have been published over recent years [78–82,84–92] and,
sory to obtain as low a density as possible in the concrete, retaining in general, it is accepted that the ITZ morphology-quality plays
the rest of its beneficial properties. In this case, a an important role in the global permeability and therefore the
‘‘slightly-lower-density EAFS’’ is desired, to decrease the concrete durability of hydraulic mixes, mortars and concretes. However,
density until it reaches values close to those obtained when using its influence on mechanical properties such as strength (tensile
natural siliceous or calcareous aggregates. The usual content of and compressive), stiffness and toughness have yet to be clearly
Fe-element in EAFS is between 20% and 30%, which implies an iron established.
oxide content of 30–45% in weight; these values can be reduced in The ITZ has been described as a zone surrounding the aggregate
the steelmaking below 15–20% in Fe-element and below 22–30% in particles and their contours of around 15–40 lm in size [80]. The
iron oxides. An additional porosity of about 5% in the EAFS will main characteristics of this zone in the hard concrete have been
contribute to a reduction in its density with no detriment in its identified as important porosity, a very high content of
properties. It appears possible to reach values of between 3 and Portlandite, a presence of ettringite, and a lack of hydrated calcium
3.2 Mg/m3 in the density of EAFS without affecting steel and slag silicates (S–C–H gel). Even the orientation of the Portlandite and
quality; in this case, the density of the resultant concrete (contain- ettringite crystals and the size of the neighbouring cement grains
ing about 1800 kg/m3 of EAFS) can be kept below 2.6 Mg/m3; 8% before the setting have been analysed. It is in fact accepted that
higher than conventional concrete. Subsequent use of suitable the conditions of the fresh concrete and its setting and hardening
air-entraining additives in mixes can reduce the density even fur- strongly influence the resultant morphology and the state of the
ther to within the range of 2.5–2.6 Mg/m3, which is a good value ITZ. Obviously, the long-term hydration of all cement particles
for the key strength-to-weight ratio of load-resistant materials. (weeks, months) and the presence of Portlandite will promote slow
and progressive changes in the morphology of this ITZ zone.
The water/binder ratio in the vicinity of the aggregate parti-
3. The use of EAFS in hydraulic mixes up until the present and cles is notoriously increased in conventional concretes, compared
some new observations to the average value in global concrete, which produces a porous
ITZ. At this point, the behaviour of the EAFS in the presence of
Analyzing the role and the influence of EAFS used as aggregate liquid water should be mentioned; in fact, there are only small
in hydraulic mixes requires some investigation of the chemical amounts of capillary water on the surface of the EAFS pieces
interaction between EAFS, water and the cementitious matrix, [81]. The ruggedness, the accessible porosity and the presence
including the presence of free-CaO. There is evidence of migration of hydrophilic (silicates) and hydrophobic (iron oxides) sub-
(diffusion of ions in aqueous solution) of this oxide from the core to stances in the external contour of the slag pieces provoke a sit-
the periphery of the aggregate pieces; periodic visual inspections uation in which capillary water exists on the surface of EAFS, but
of a stock-pile of EAFS exposed to weathering recorded changes not in abundance, and there is no bleeding due to gravity. The
in colour of the external surface material (associated with rainfall ‘‘wall effect’’ of common aggregate pieces, whether siliceous or
and its evaporation), from grey-black to grey-white. The white sub- calcareous, which produces an anomalous packing of cement
stance on the external surface was clearly calcium carbonate. The particles in the vicinity of their surfaces, might be minimized
following was observed in relation to the migration of CaO. in the vicinity of EAFS pieces. An ITZ depleted of large cement
Two relevant factors should be considered. Firstly, EAFS is grains and with a scarce presence of small grains, is not evident
gravel-like material the pieces of which contain pores, cracks and in the EAFS aggregates, the surfaces of which do not repel the
crevices from occluded gases in a liquid state at high temperature, cement particles because of their similar components (silicates
variations in volume throughout cooling, the crushing process, and and oxides).
the initial hydration of the accessible free-CaO due to rainwater. Therefore, the ITZ created in mixes that contain EAFS (in well
Secondly, the dissolution of natural calcite that gives us the performed mixes, with low effective water-to-cement ratios) at
well-known geological forms of stalagmites and stalactites can the end of the setting period, should differ from that of concretes
explain the migration observed in EAFS stock-piles: accessible cal- that contain ordinary aggregates; this ‘‘new’’ ITZ will be smaller
cium oxide (free-CaO) added to rainwater and atmospheric carbon and less hollow than it is with natural rock aggregates. The slow
 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79 71

migration of CaO from the core of the EAFS pieces to its surface, It was concluded that the ITZ explains the inelastic (non-linear)
and its subsequent chemical evolution to calcium carbonate, also behaviour of concrete under loading–unloading cycles in compres-
affects the ITZ morphology. Hence, variations in the morphology sion tests [82], despite the fact that the present phases, aggregates
and age-evolution of the ITZ around the EAFS pieces may be and matrix, show a separate linear behaviour. Certainly, the stress–
expected, accompanied by variations in the global properties of strain graph obtained with standard concretes tested under com-
the concrete, such as its permeability, durability, and mechanical pression to failure shows a decreasing slope. However, when the
properties (tensile and compressive strength and stiffness). EAFS mixes were tested under compression to failure, an
The fracture surfaces of concrete specimens after mechanical almost-linear-elastic behaviour was observed in the load–strain
tests, in which the larger aggregate pieces have detached them- graph [82]; hence, this effect is probably a further consequence
selves from the matrix, are widely accepted to be undesirable; on of a singular ITZ, when the mixes are well-graded and they show
the contrary, when fracturing breaks and divides these coarse high performance.
aggregate particles in a visible way, showing good adherence and Finally, it should be stated that significant changes in the mor-
cohesion between matrix and aggregate, the situation is encourag- phology of the ITZ will give rise to changes (although none too
ing. Some authors [81,82] have observed a generally lower drastic) in the global properties of the concrete; as was observed
strength of the global concrete than of its components, aggregates in this case study.
(calcareous or siliceous) and cementitious matrix; they have
explained this observation by a specific low-strength in the ITZ. 4. Materials
Hence, it may be stated that the better the quality of the bond in
the ITZ, the better the mechanical (tensile and compressive) 4.1. Cement, water and natural aggregates

strength of the concrete. In general, the concrete made with EAFS A Portland cement type I, as per ASTM C150 standard [94] with a chemical com-
shows broken aggregate particles on the fracture surface after position and particle fineness commonly found in ordinary concretes was used in
mechanical rupture testing, which is an evidence of a stronger this work. Mixing water was taken from the urban supply of the city of Bilbao,
ITZ; however, it should also be considered that the EAFS pieces which showed a negligible amount of compounds that could affect the preparation
of hydraulic mixes.
have cracks and crevices in their mass, favouring breakage under
Siliceous fine aggregate of washed sand (from Arija to Burgos), sized between
lower loads. 0.1 and 1 mm with a fineness modulus of 1.36 was used. The quartz particles were
Some studies [78,81,82] concluded that the porosity of the ITZ rounded, as revealed by the SEM images of mixes, with a specific gravity of
and the micro-cracks that extend out from the ITZ towards the 2.63 Mg/m3.
cementitious matrix were the origin of general cracking in the con- Limestone aggregate, crushed and classified in three sizes (fine 0–5 mm, med-
ium 5–12 mm and coarse aggregate 12–25 mm) was used. The chemical and phys-
crete under strong external loading. This micro-cracking has fre- ical characteristics are detailed in Table 1, and the specific gravity was 2.67 Mg/m3.
quently been observed in ordinary concretes under SEM
microscopy and is attributed to differential deformations between 4.2. Electric arc furnace slag
aggregate and matrix under stresses, thermal variations and drying
shrinkage. The aforementioned investigations stated that the exis- Two types of crushed electric arc furnace slag (EAFS1 and EAFS2) were used in
this study, as detailed in [35], supplied by two different steelmakers. Some images
tence of this interconnected and generalized micro-cracking can
of EAFS1 (fresh and after long-term weathering) are shown in Fig. 1. Their global
affect the mechanical strength of the mass of concrete and its chemical composition and physical properties are detailed in the Table 1 and their
transport properties. grading followed the method described for the limestone aggregate. The slag sam-
The microscopic observations performed on EAFS mixes ples from the steelmaker that produced the EAFS2 underwent slower cooling with
recorded no micro-cracks in the cementitious matrix surrounding greater evacuation of gases that resulted in lower porosity and water absorption,
but with a higher specific gravity, unlike the EAFS1 slag that underwent a slightly
the slag particles, though these particles show internal cracking;
different production process. Other factors that have an influence on slag density,
these EAFS concretes are, in general, less permeable than ordinary such as the proportion of iron oxides and the metallic iron content, were similar
concrete [81]. When observations were conducted on the fracture in both slags. The results of X-ray diffraction in relation to the main crystalline com-
surface of broken EAFS concretes after mechanical tests, only a few ponents of the slag are also shown in Table 1.
large cracks were observed, and the main crack broke the aggre-
gate particle. No bleeding was noted by the authors of this study 4.3. Concrete preparation

in the larger-sized concrete particles (larger than 1 mm) prepared Three concrete mixes were prepared, one of which was a reference concrete CR
with EAFS aggregate, nor has bleeding been noted in the literature made using natural aggregates (crushed limestone and a minor proportion of silic-
[81,93]. eous sand), and the other two mixes had the same proportion of siliceous sand and

Table 1
Chemical composition (XRF) and other physical properties of aggregates.

Aggregate EAFS1 EAFS2 Limestone

Fe2O3 (%) 30.8 27.54 0.34
CaO (%) 32.52 25.72 51.68
SiO2 (%) 17.17 17.88 3.54
Al2O3 (%) 7.96 11.62 2.52
MgO (%) 4.56 3.82 0.64
MnO (%) 3.8 4.15 –
SO3 total (%) 0.25 0.01 0.39
Na2O + K2O (%) 0.2 0.1 0.25
P2O5 (%) 0.58 0.46 –
TiO2 (%) 0.59 0.71 0.05
Loss on ignition (%) – – 42.30
Porosity (%) 14.4 7.8 0.7
Water absorption (%) 7.37 3.35 0.52
Specific gravity (Mg/m3) 3.01 3.32 2.67
X-diffraction main compounds Wustite-magnetite Wustite-magnetite Calcite-dolomite minor
Ghelenite-Kirschsteinite(Mn), Larnite-Ghelenite
Chromite Chromite
72 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79

5. Results of the EAFS characterization

The observation and analysis by means of SEM and EDX

micro-analysis of polished samples of the hydraulic mixes,
included in the following sections, provide relevant information
on the structure and components of the EAFS in this study. Some
images that illustrate the morphology of these components are
shown in Fig. 2.
Samples of the slags were used to evaluate their dimensional
stability in several states: as received without aging, after a period
of three months of natural aging exposed to weathering and, finally
after a period of more than five years in outdoor conditions. The
tests were performed as per the ASTM D-4792 standard [94], sub-
merged in water at 70 °C for over 2000 h, and the results are shown
in Fig. 3, with logarithmic ordinates for the sake of clarity. The
results of potential expansiveness in the EAFS1 indicate an
indispensable aging-weathering treatment of over two or three
months for reliable use of this slag in the manufacture of concrete
Fig. 1. Fresh and long-term weathered EAFS1 slag. (expansion below1%). However, an eventual treatment similar to
that proposed for EAFS1 slag is unnecessary for EAFS2 slag, as its
expansion was under 1% in its ‘‘fresh-as received’’ state.
Table 2 Furthermore, thermo-gravimetric and differential scanning
Characteristics of the concrete mixtures. calorimetric tests were performed on the samples after the afore-
Mix design CEAFS1 CEAFS2 CR mentioned accelerated test. Fig. 4 shows the results of these tests.
CEM I 52,5 R (kg/m3) 300 300 300
As expected, the content of free-CaO in slags EAFS1 and EAFS2 was
W/C 0.69 0.65 0.59 different and may be estimated at 2.5% in slag EAFS1 and at 0.2% in
Slump (mm) with 3.5% additive 210 200 210 slag EAFS2. These estimates following hydration and carbonation
Fresh density (Mg/m3) 2.8 2.96 2.51 and de-hydration and carbonate decomposition at 900 °C are
Hardened density (Mg/m3) 2.53 2.73 2.36 largely reliable.
Compressive strength at 28-days (MPa) 55.0 55.7 40.8 SEM observation and EDX analysis of both kinds of slag particles
Compressive strength at 90-days (MPa) 62.8 60.1 57.3
showed the appearance of the different compounds or phases pre-
Porosity by MIP (%) 11.9 10.1 9.6
viously revealed in the XRD analysis. In Fig. 5, the main compounds
and the mapping of chemical elements throughout the image may
be seen in slag EAFS1; a similar observation is shown in Fig. 6 for
two kinds of EAFS as aggregates, with the same grading and proportions as the
limestone aggregate. Table 2 shows the main characteristics of these mixes, EAFS2 slag. Aluminium, Iron and Chromium are the most signifi-
detailed, and discussed in a recent publication [35]. cant elements to identify the present phases.
The matrix characteristics of these three mixtures, excluding the fine and coarse
aggregates, should be the same, because their design is meant to be as similar as
possible: the same cement content, the same fine fraction and water, similar plas- 6. Results of the ITZ analysis
ticizer additives and the same volume and grading of coarse aggregate. The differ-
ences in the measured porosity analyzed by Mercury Intrusion Porosimetry (MIP) 6.1. SEM-EDX analysis
should come from the fine fraction of the EAFS included in the small samples.
Physical and mechanical tests were performed on these concretes yielding
results that may be found in [35]; it should be added that the compressive strength Following a detailed observation by SEM and the additional use
after one year (long-term) reached a convergent value (about 62–65 MPa) for all of of EDX-microanalysis of the hydraulic mixes made with EAFS
the concretes in this study. In the present article, an analysis of the EAFS particles aggregate, outstanding differences were observed in the
and the ITZ found in these mixes is presented. Interfacial Transition Zone (ITZ). According to the literature [70],

Fig. 2. EAFS1 (upper) and EAFS2 (lower). The bands are one centimeter in length.
 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79 73

Fig. 3. Graph of slag expansiveness after ASTM D-4792 standard test.

Fig. 4. TG-DSC graph of slags.

74 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79

Fig. 5. EAFS1 microstructure and internal distribution of several chemical elements.

the ITZ has an extension of around 15–30 microns from the parti- showed contours detached from the surrounding cementitious
cles surface, but in the SEM image, Fig. 7, a dark (black) ‘‘capillar matrix and the appearance of the concrete in these areas, border-
y-hole-crevice’’ with a width of 2–4 microns is visible along the ing the limestone and the sand zones, was very similar to the
contours of the natural aggregate particles. appearance of the external surfaces of the set concrete (wall effect).
In this Fig. 7, a particle of quartz-sand and another particle of In contrast, the pieces of slag were broken on the fracture surface;
EAFS1 are separated by the cementitious matrix in concrete which is once again quite logical, because the interfacial adherence
CEAFS1; some internal cracks are visible in the slag particle. A with the matrix was better and the internal cracks assisted their
more extended black hole-crevice may be seen in the contour of breakage.
the sand particle than in the contour of the slag particle, in A relevant image of concrete CEAFS2 is shown in Fig. 8. None or
which some regions of its contour reveal no visible border only a few holes may be observed in some zones of the slag particle
(right-hand-side image) around the cementitious matrix. An image contour (left); the border areas are full and fairly adherent. The
analysis program even makes it possible to evaluate the ratio most prominent detail is a band surrounding the slag aggregate
length of the black hole-crevice-ITZ versus total contour length, which has the same grey shade as most of the smaller particles
for both kinds of particles; the numerical result is 78% in the sand on the right; these smaller particles are fine-limestone aggregate.
particle and 32% in the slag particle. These values are the average The EDX analysis revealed a band of almost-pure calcite with a
from the measure of that ratio in three particles of each kind, sand width of 15–20 microns; as previously explained, this calcite is
and slag, in the two type of concrete. mainly from the free CaO of the slag. It could even partially come
It appears logical, on the basis of these observations, to think from the Portlandite, produced by the Portland cement, present
that about 78% of the external surface of the sand pieces have in the vicinity of the cementitious matrix in the region of the ITZ,
almost-null adhesion to the surrounding cementitious matrix; a although this source is neither proven nor verified.
value that is, on the contrary, far lower (32%) for the slag particle. The situation described in Fig. 8 for the CEAFS2 is repeated in
The mechanical tests on this concrete yielded consistent results: on the SEM micrographs of concrete CEAFS1. It is more frequent in
the fracture surface, the limestone and the sand-quartz pieces CEAFS1, as EAFS1 contains more free-CaO than EAFS2. However,
 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79 75

Fig. 6. EAFS2 microstructure and internal distribution of several chemical elements.

Fig. 7. CEAFS1 microstructure (left). Image analysis of porosity in black colour (right).

the presence of calcite is only found on a small fraction of the con- 6.2. Ultra-micro-indentation tests
tours of the slag particles and is not continuous along all particles.
Finally, the ITZ in the reference concrete CR is shown in Fig. 9, in Ultra-micro-indentation tests (Shimadzu DUH-211) were per-
which aggregate particles of siliceous sand and limestone are com- formed on a concrete sample in the vicinity of the EAFS aggregate
pared; in the second image the contours of both of these aggre- particles. A charge of 5N was used on a micro-indenter to obtain
gates can be clearly observed, only a few of which are coherent indentations of 1–5 microns. The indentation footprints were per-
with the cementitious matrix. Several hundred SEM images of all formed on a slag contour region in which the ITZ
these concretes were taken in the course of this research and those black-hole-crevice was almost inappreciable. The traces and the
included in this article are illustrative examples. microstructure of the slag aggregate and the cementitious matrix
76 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79

Fig. 8. SEM image of the microtexture of concrete CEAFS2.

Fig. 9. SEM image of the microtexture of reference concrete CR.

were difficult to perceive in the optical microscopy images. The the aggregate particles. In our case, the fall in hardness can be
values obtained are shown in Table 3. appreciated in the zone close to the slag particle contour (hole)
Doubts persist over the use of micro or nano-hardness values in which values are slightly under 200 MPa; from a distance of
measured in a hollow-creviced region or in very porous region. 5–20 microns the values are almost-constant, and homogeneous
Other authors [74,76] have published works in which such values values of around 300 MPa are only measured in the matrix at a dis-
are fixed and are represented in graphs in terms of the distance to tance of over 25 microns. Comparing these results with those
 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79 77

Fig. 10. Elastic moduli of the concretes.

Table 3
Table 4
Hardness values in MPa, measured from a slag particle to the cementitious matrix.
Strength values of the concrete.
Distance Slag 1–2 lm 5 lm 10 lm 15 lm 20 lm 25 lm
Mix design CEAFS1 CEAFS2 CR
from slag aggregate
aggregate Compressive strength at 28-days (MPa) 55.0 55.7 40.8
Compressive strength at 90-days (MPa) 62.8 60.1 57.3
Series 1 1151 187 220 238 241 275 312
60% Compressive strength at 90-days (MPa) 37.7 36.1 34.4
Series2 1034 194 212 245 245 245 295
Elastic modulus at 28-days (GPa) 40.5 39.6 41.7
Series3 825 254
Elastic modulus at 90-days (GPa) 42.2 41.8 44.0
Distances in lm are measured from the contour of the particle to the surrounding
matrix.

90-day compressive strength, assuming that the highest in-service

obtained in the literature, it was concluded that the ITZ quality stress of this material in a structure is around that value (see
around the slag particles was excellent, and that the affected zone, Table 4).
within a radius of 25 microns, showed good level of hardness A good quality ITZ enhances the global elastic modulus and the
(240 MPa) compared to the hardness of the cementitious matrix. straight linearity [81]. The results showed a good linearity within
the range of in-service loading for the EAFS slag concretes; the ref-
6.3. Compressive tests erence concrete showed a small decrease in the slope of the curve
at higher stress values could be attributed to a lower quality ITZ
Load-unload tests were performed on the concrete mixes to that was subsequently affected by micro-cracking. However, the
estimate the elastic modulus and the linearity of the stress–strain values of the elastic moduli are slightly smaller in the EAFS con-
relationship (see Fig. 10). The maximum load level was 60% of the cretes than in the reference concrete.
78 I. Arribas et al. / Construction and Building Materials 90 (2015) 68–79

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