MRS Advances © 2018 Materials Research Society

DOI: 10.1557/adv.2018.186
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Waste Steel Slag and their Influence on the Properties of Cement Blends

Sunday O. Nwaubani

School of Civil and Environmental Engineering, University of the Witwatersrand, Johannesburg,

Sought Africa.

ABSTRACT

The use of waste is rapidly becoming a supra-disciplinary field in most parts of the world where
the use of industrial wastes like fly ash, granulated steel slag, silica fume, and waste fibers in
construction has become very popular since the last half of the 20th century. Other forms of
industrial wastes are also re-used even for more sensitive applications on soils to upgrade soil
texture. For example, waste from bauxite refining (red mud) is known to be extensively re-
utilised. These concepts are yet to take tangible hold in Africa, despite the huge resources
available. Electric-Arc Furnace Steel slag is a major waste product from the steel industry
involving the melting of scrap to make steel in an electric arc furnace. Use of such waste
materials in construction alleviates the huge environmental pollution problem which often exists
in areas where they are produced and/or dumped. Currently, the material is mainly used in
construction works as unbound aggregate for asphalt concrete pavements, or as road base in
many countries. However, it consists predominantly of oxides and silicates of magnesium,
calcium, aluminium, iron and thus can be used as substitute for cement. This paper compares the
effect of utilising this type of Steel slag and Granulated Blast Furness Slag, as partial
replacement for Portland cement. The influence of the physical and chemical characteristics of
the two materials on the setting time, compressive strength, total porosity and pore-size
distribution of cement pastes have been evaluated. For the experimental conditions studied, the
result reveal adequate properties for high levels of replacement but suggests that superior
qualities, compared with Portland cement concrete is possible only if replacement levels do not
exceed about 10%.
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INTRODUCTION

It is now well established that good quality and durable concrete may be produced using
supplementary cement materials. The main types of these materials, which are widely used in
many developed countries, include Fly Ash, Micro-silica, Meta-kaolin and Ground Granulated
Blast Furnace Slag (GGBS) [1,2]. None of the cement supplementary materials mentioned
above are produced in Libya; however, the country produces more than 27,000 tons per annum
of Electric Furnace Steel Slag as a major waste by-product of its iron and steel industry [3],
before the recent political upheavals. The Libyan Iron & Steel Co (LISCO) has a design capacity
of 1,324,000 tons of liquid steel, and with around 6,500 workers, it is the largest employer in
Libya [4]. With only four of its six electric arc furnaces now back in operation after the war, the
company produced almost 50,000 tonnes of steel in 2012, as reported by Libya Business News
on 12 February 2013. The main waste resulting from this industrial activity is steel slags which
get deposited in the surrounding areas causing enormous environmental pollution. The
cementing properties of Electric Furnace Steel Slag has been investigated and confirmed by
many researchers [5, 6]. They are also known to have good binding properties which may result
in technical, economical, and environmental advantages over conventional cements [7]. There is
therefore a need for an in-depth investigation of the properties of this material when used in
cement systems as the importance of resource efficiency through use of this waste material in
producing good quality and durable concrete cannot be over-emphasised for developing
countries like Libya, where the estimated need for urban housing stands at about 900,000 extra
housing units. According to an exclusive interview granted to the Libyan Herald in 2012, the
Chairman of the Libyan Housing Authority observed that, although there are several thousand
housing units available, they are not enough to meet the demand of over 100,000 units per
annum.
The study described in this paper is part of a more comprehensive feasibility study
carried out to assess the potential use of this waste slag as a partial replacement for Portland
cement. Various possibilities are being investigated, however, the results presented here relate
only to the influence of substituting Portland cement with waste electric-arc furnace slag on the
setting time, compressive strength, total porosity and pore-size distribution of cement paste
mixtures. The results are compared with those obtained for mixtures containing GGBS, which
has a good track record as a substitute for Portland cement in concrete.

MATERIALS

Source and characteristics

Three cementitious materials were used in this study; Portland cement (PC), Ground
Granulated Blast Furnace Slag (GGBS) and Air-Cooled Electric-Arc Furnace Steel Slag
produced in Libya (LSS). The physical and chemical characteristics of these materials are
described below and presented in Table 1 and 2 respectively.
The cement used was a commercial product designated as Portland cement class 42.5
which complies with BS EN 197-4:2004 and supplied in the UK by Blue Circles Cement
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Limited. The GGBS used complied with BS EN 197-1:2011 and was supplied in the UK by
Civil and Marine Slag Cement limited.
The LSS used was a non-commercial air-cooled electric-arc furnace steel slag produced
in Libya as a by-product of the Iron and steel industry. The slag was initially supplied in form of
medium size (100 to 400mm) rocks that were then crushed down to smaller pieces in the
laboratory using a Kanga Hammer. The broken pieces were then sent to the local Cement
Company to be ground into a powder size comparable to that of PC. Finally, the slag was sieved
to pass through a 600µm sieve, in order to remove any remaining larger particles.
The physical and chemical characteristics of the PC, GGBS and LSS were assessed using
standard laboratory techniques and specifications. The characteristics determined were, relative
density, specific surface area, particle-size distribution, glass content and loss on ignition. The
technique used and the results are presented in Table 1 and 2 and discussed below.

Relative humidity

The relative densities of the starting materials were determined using Helium Auto-
Pycnometry Technique. The method employs the ideal gas law to measure the solid volume of
the sample taking advantage of the fact that Helium gas flows rapidly into most pores without
interacting with the active components of the cement binder in the sample. Knowing the mass,
and the volume of the sample, it was possible to then calculate the relative density.
Approximately 10g of the samples investigated were first oven-dried at 110oC until a constant
mass was achieved. The density of the material was measured by placing a pre-weighed test
sample in the sample chamber of a Helium Auto-Pycnometer, (Model 1330 V1.02), which has a
sample chamber and an expansion chamber of known volumes and equipped with a computer.
During the test, Helium under pressure is admitted into the sample chamber and fills the sample
chamber as well as the pores in the test sample to a known pressure. The sample chamber is
then connected to the expansion chamber, which is at ambient pressure. Following this, the
helium moves into the expansion chamber, and the pressures of the two chambers equilibrate to
an intermediate value. Since the volumes of both chambers and the gas pressure are known, the
skeletal volume of the test sample can be calculated by the associated computer. The results are
shown in table 1.

Specific surface area

The Specific Surface Area, SSA, was measured using the BET Nitrogen Adsorption
method described by Brunauer et al [8]. Certified external testing houses (Micromeritics) carried
out these determinations and are shown in Table 1 above. It can be seen that the SSA of the LSS
falls between that of the GGBS and PC, therefore the grinding and sieving process employed
produced a material of acceptable SSA in comparison with commercially produced cementitious
materials. The results presented in table1 also show that the SSA of the GGBS was higher than
that of the LSS. This could imply that further grinding of LSS may be beneficial in improving its
reactivity.
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Particle size distribution

The particle size distribution of the test materials were measured using a Malvern
instrument (Laser diffraction particle-sizer, series 2600c Master-Sizer). Neville [9], have
established that early strength development of concrete is better if at least 50% of the PC
particles lie between 3 and 30µm, with correspondingly fewer very fine and very coarse
particles. The results obtained from this study shown below in table 1 indicates that the
percentage of particles that lie within this range were 62.5, 76.4 and 56.8 for PC, GGBS and LSS
respectively. The result also show that LSS used for this study has a greater amount of particles
larger than 102 µm (1.2%) but GGBS (0.1%) and PC ( 0%). The presence of these larger
particles in the LSS would affect its reactivity negatively.

Table 1. Physical Properties of the cementitious materials used

Physical Properties
Property PC GGBS LSS
Colour Grey White Dark
Grey
Relative Density (g/cc)* 3.18 3.025 3.61
SSA (m2/kg)** 985 1571 1358
Glass Content (%)** - 98 57
% of particles between 3 and 30 µm.*** 62.50 76.40 56.8
Glass content (%)**** - 98.00 57.0
Loss on Ignition (%)***** 1.30 1.07 0.53

* Helium Auto-Pyconometry, **BET Nitrogen Adsorption, ***Malvern Laser diffraction,

****X-Ray diffraction (XRD), *****X-Ray Fluorescence (XRF).

Chemical oxide composition

The analysis for the chemical oxide composition was determined using X-Ray
fluorescence (XRF) technique. The results are presented in table 2 and reveals that the main
oxide compositions common to all of the three materials under study are CaO, SiO2 and AL2O3.
These oxides play a major role in determining the reactivity of the materials. The steel slag has a
comparatively higher amount of iron oxide (Fe2O3) content, 19.51%, when compared to 2.74%
and 0.80%, for the PC and GGBS respectively. The high iron content is a typical characteristic of
steel slag and is one of the main reasons why they are not commonly used as cement
replacement materials[10] LSS has very low sulphur content(less than 0.05%). BS EN 15167-
1:2006 specifies that the SO3 content in slags should be no more than 2.5%. The magnesium
oxide content for LSS is 14.31%, which is slightly higher than the 14% maximum specified in
BS EN 15167-1:2006. When the proportions of the compounds present in the GGBS and LSS are
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compared, it can be seen that both contain similar proportions of CaO and that both are low in
SiO2 and high in MgO. The interaction between these compounds is very complex and cannot be
easily summarised. However, it is the ratios in which these compounds are present that may
affect the usefulness of LSS as a cement replacement material. The (CaO + MgO)/SiO2 was 3.11,
which is significantly greater than the minimum value of (1.0) specified in BS EN 15167-1:2006,
and so should not hinder the use of LSS as a cement replacement material. Also, the alkalinity
factor described by Wu et al[11] as (CaO/SiO2 + P2O5), for LSS is 2.19. This is greater than the
1.8 minimum specified by WU et al [11] as crucial in order for steel slag to be used as a cement
replacement material. On the negative side, the (CaO)/(SiO2) ratio was 2.25, which is greater
than 1.4 specified in the code. This is greater than the 1.8 minimum identified by Wu et al [11],
as being crucial for a material to be used as replacement for cement in concrete. Taken together,
the implication of higher (CaO)/(SiO2) ratio, high MgO content (see Table 2) and the presence of
coarser particles, is a greater possibility of concrete unsoundness occurring when LSS is present
as a cement replacement material [12].

Table 2. Chemical Oxide Composition of the Cementitious Materials used.

Chemical Oxide
Composition
Compound PC GGBS LSS
(%) (%) (%)
Silica (SiO2) 20.3 35.61 16.76
Alumina (Al2O3) 5.04 12.21 6.11
Lime (CaO) 64.8 40.21 37.76
Ferric Oxide (Fe2O3) 2.74 0.80 19.51
Magnesia (MgO) 1.02 8.80 14.31
Sulphur Trioxide(SO3) 2.92 1.94 <0.05
Potash (K2O) 0.68 0.46 <0.01
Soda (Na2O) 0.11 0.16 0.16
Titania (TiO2) 0.28 0.55 0.93
Phosphorus Pentoxide (P2O5) 0.11 <0.02 0.47
Chromium Sesquioxide (Cr2O3) 0.21 <0.01 0.10
Manganese Oxide (Mn2O3) 0.07 0.46 2.45
Zirconia (ZrO2) <0.0 0.03 0.04
Hafnia (HfO2) <0.0 <0.01 <0.01
Lead Monoxide (PbO) <0.0 <0.02 <0.02
Zinc Oxide (ZnO) 0.01 <0.01 <0.01
Barium Oxide (BaO) 0.02 0.11 0.05
Strontia (SrO) 0.16 0.08 0.02
Stannic Oxide (SnO2) <0.0 <0.01 <0.01
Stannic Oxide (SnO2) <0.0 <0.01 <0.01
Cupric Oxide (CuO) <0.0 <0.01 <0.01
Loss on ignition(LOI) 1.37 1.07 0.83
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EXPERIMENTAL DETAILS

Mixture proportions and curing

The various cement paste mixtures used in this study were prepared with constant binder
content and a free Water/binder content of 0.4. Distilled water was used in preparing all mixtures
used in the investigation. A simple approach has been adopted which involves partial
replacement of the normal Portland cement used in the control samples (Mixture O), with an
equal weight of GGBS (Mixture G) or Libyan slag (Mixture LS). The levels of Portland cement
replacement were 10%, 30% or 50%. Table 3 summarizes the mix proportions (by weight) for
the various mixtures investigated. After mixing, samples were left to cure in a fog room,
maintained at a constant temperature of 20°C +/- 2°C and 99% relative humidity until tested.

Table 3. Mixture Proportions

Notation Mixture Proportion (% by weight)
PC GGBS LSS Water/Binder
O 100 - - 0.4
10 90 10 - 0.4
30 70 30 - 0.4
50 50 50 - 0.4
10 90 - 10 0.4
30 70 - 30 0.4
50 50 - 50 0.4

Setting times
The setting times for the various cement paste mixtures were determined using the
standard Vicat test technique as described in BS EN 196: Part 3: 1995[10].

Compressive strength

The compressive strength development for all cement paste mixtures were measured using
100mm cubes in a crushing machine, in accordance with BS EN 12390-3:2009, 2009
specifications. Tests were conducted on samples cured for 3, 7, 28, 180 and up to an age of 365
days as shown in Figure 2.

Total Porosity and Pore-size Distribution

The total porosity was measured using mercury intrusion porosimetry (MIP) technique.
The MIP technique measures the volume distribution of pores in the materials by mercury
intrusion at very high pressure. Mercury is ideal as an intrusion liquid as it has a high surface
tension and it does not wet or react with most materials. MIP gives a very good picture of the
size of the pores and their distribution within the paste matrix. The equipment used was supplied
by Micromeritics [13].
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RESULTS AND DISCUSSION

Setting-time.

The initial and final setting times (I. S. and F. S. respectively) for the control mixture
(100% Portland cement) and those containing 30% Portland cement replacement (Mixture 30G
and 30L) are presented in Figure1 below. These results were recorded to the nearest 5 minutes
and are presented as the average of two values. The initial and final setting times for mixtures O,
30G and 30L when compared, revealed that the replacement of 30% of the normal Portland
cement increased the setting times. Similar behaviour has also been reported for mixtures
containing GGBS by the ACI committee report266 1R-1987[14], and the Concrete Society,
Technical Report No. 40, 1991[15]. The extended setting time for these mixtures gives an
indication of slow chemical reactivity of the constituent cement replacement materials. This in
turn is mainly because cement replacement involves a reduction in the major chemical
compounds which affect the speed of hydration.

400

300

200

100

0
30 G

30 L
O

M ix

Figure 1 setting times for paste mixtures

Compressive strength

. The experimental results are presented in Fig. 2 as the average of 3 values. The results
show that the ultimate strength obtained for mixtures containing GGBS at 365 days was higher
than that of the control mixture (100% normal Portland cement), whereas, the strength at all ages
for mixtures containing 30 or 50% LSS was lower than the control. For 10% LSS replacement,
the compressive strength was lower than the control at early ages but quite like the control after
long-term curing.
Fig. 3 shows the influence of GGBS additions on compressive strength when the results
are presented as a percentage of the strength of the control mixture of the same age. Between 3
and seven days, the rate of strength gain observed for the GGBS mixtures was lower than that of
the control. At 28 days the strength of all mixtures containing GGBS was similar to that of the
Control mix. However, at 180 and 365 days the strength of all mixtures containing GGBS was
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higher than that of the control mixture. This increase in strength was approximately proportional
to the level of normal Portland cement replacement and are consistent with those reported by
other researches [15,16].
Compressive Strength ( MPa)

Age (days)

Figure 2. Compressive strength development for cement paste mixtures

Relative Compressive Strength (%)

O
10G
30G
50G

Figure 3. Relative compressive strength of cement paste mixtures containing GGBS

The influence of LSS addition on the strength results is shown in Fig. 4. The results are
again presented as a percentage of the strength of the control mixture at the same age. This
decrease was proportional to the level of normal Portland cement replacement at ages of 3 and 7
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days. However, at ages of 28 days and above, the reduction of strength was less than would be
suggested by the proportion of normal Portland cement replacement. This is illustrated by the
relative strength of mixtures containing 30 or 50% LSS reaching 94% and 80% of the strength of
the control respectively at an age of 365 days.
Relative Compressive Strength (%)

Figure 4. Relative compressive strength of cement paste mixtures containing LSS

Total Porosity and Pore-size distribution

Table 4 presents the cumulative volume of pores intruded (total porosity) obtained from
the MIP test for mixture O, 30G and 30L when cured up to an age of 180 days. The results show
that there was a reduction in porosity with age for all mixtures. At 7 days, the porosity of the
mixture containing 30% LSS (Mixture 30) was much higher than that of the other mixtures,
however, at later ages, its porosity approached that of the normal Portland cement control
mixture. Conversely, mixture containing 30% GGBS had the lowest porosity at all ages.

Table 4. Total Porosity.

Total Porosity=Cumulative volume of pores intruded(ml/g)
Age (Days) Mixture O Mixture 30G Mixture 30L

7 0.70 0.16 0.24

28 0.60 0.15 0.19
180 0.12 0.11 0.16

Figures 5, 6 and 7 show the pore size distribution for the various cement paste mixtures
when cured up to an age of 180 days. All the results show a decrease in the total volume of pores
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with age. The results show that the presence of GGBS resulted in a finer pore-size distribution
and lower total porosity. Conversely, mixtures containing 30% LSS had a larger pore volume
and a correspondingly coarser pore-size distribution. The same general trend is represented for
these mixtures at 180 days (Figure 8).
Cumulative Volume (ml/g)

----7 days
0.15
----28 days
----180 days

Figure 5. Pore size distribution for Mixture O (100% PC).

----7 days
Cumulative Volume (ml/g)

----28 days
----180 days

Figure 6. Pore size distribution for PC/GGBS blend

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----7 days
----28 days
----180 days
Cumu l a tive Vo l ume (ml / g)

Figure 7. Pore size distribution for Cement/(30% L) blend.

O
30G
Cumulative Volume (ml/g)

30L

1.000
Pore Radius (µ)

Figure 8. Pore size distribution for the different paste mixtures at 180 days.

A typical pore size distribution for hardened cement encompasses a large range,
extending from about 10 µm to as small as 0.5 nm or less in diameter. The larger pores, ranging
from 10 µm to 10 nm, are the residual unfilled spaces between cement grains, categorized as
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capillary pores. The finest pores, ranging from approximately 10 nm to 0.5nm, are called gel
pores since they constitute the internal porosity of the C-S-H gel phase. It had been established
that irrespective of the age of hydration and the Water/Cement content, as long as hardened
cement paste does not contain pores greater than 132 nanometres, its permeability would remain
insignificantly low [17,18,19,20]. In this investigation, the cumulative volume (ml/g) of pores
greater than 0.10µm (100 nanometre), for the different cement paste mixtures is presented in
Table 6.

Table 6. Total volume of pores (ml/g) greater than 0.132µm.

Total volume of pores (ml/g) greater than 0.132 µm.

Age Mixture O Mixture Mixture
(Days) 30G 30L
0.103 0.065 0.144
28 0.033 0.022 0.085
180 0.007 0.007 0.022

These results follow a similar trend to that observed for the total porosity (Table 5). It
suggests that the long-term pore-size distribution of the mix incorporating 10% LSS is very
comparable to that of the control PC mix. This is also evident from considering the volume of
pores greater than 132 nanometers on the MIP results. The pores in mixtures containing 30%
LSS (Mixture 30L) was considerably higher than the corresponding control mixtures (Mixture
O) at all ages. This larger pore structure helps to explain the lower strengths observed for the
LSS mixtures and may have a correspondingly negative implication for their permeability
characteristics.

CONCLUSIONS

The following main conclusions may be drawn from the data presented and discussed
above:

• The setting times for mixtures containing GGBS or LSS is higher in comparison with the
control mixture. This is indicative of a slower rate of reaction of the GGBS and LSS used
and due to the reduced presence, in the mixtures studied, of the main active components in
cement responsible for fast rate of reaction and early strength gain.

• The short-term compressive strength results for mixtures containing 10% LSS is lower
than that of the control mix. However, the mix was able to achieve similar or higher long-
term strength as the control PC mix.

• The strength at all ages for mixtures containing 30 or 50% LSS was lower than the
control. For 10% LSS replacement, the compressive strength was lower than the control at
early ages but quite close to the control strength at later ages.
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• The compressive strength of specimens incorporating 30 or 50% GGBS although less than
that of the control mixture at early ages, showed higher rates of strength development at
later ages. The LSS specimens had lower strength values at both early and later ages for
this level of substitution.

• The pore characteristics study revealed the difference in the internal microstructure of the
mixtures studied. It was established that the partial replacement of normal Portland cement
with GGBS generally reduced total porosity and resulted in a finer pore structure.
Conversely, the presence of LSS resulted in a comparably higher pore volume at early ages
which is characterised by a coarser pore structure and pore-size distribution. However, the
porosity of the LSS mixtures decreased with continued curing and was observed to attain
similar values as the control Portland cement mixture after long-term curing for specimens
where the level of substitution does not exceed 10%.

• Overall, it would seem fair to conclude that the optimum replacement level for the LSS is
about 10% or less. When a greater level of substitution is used although the later age
properties of the mixtures containing steel slag may be acceptable, the slow reactivity at
early ages may give rise to low compressive strength and higher porosity.

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