Construction and Building Materials 409 (2023) 134049

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Performance of mortar and concrete containing artificial aggregate from

cold-bonded sulphidic mine tailings
Yury Villagran-Zaccardi *, Liesbeth Horckmans , Arne Peys *
Sustainable Materials Unit, Flemish Institute for Technological Research (VITO), 2400 Mol, Belgium

A R T I C L E I N F O A B S T R A C T

Keywords: Repurposing sulphidic tailings in construction products offers a sustainable solution for this mining waste. Ag­
Sulphidic mine tailing gregates (1–4 mm and 2–8 mm) were produced at pilot scale using cold granulation with minimal cement
Artificial aggregates content (6 wt% CEM III/B + 94 wt% tailings). Superplasticizer dose was optimized in mortar and concrete mixes
Cold granulation
replacing 17 % and 32 % of natural aggregates. The concretes benefit from the additional buffering capacity from
Secondary raw materials
cement hydrates in granules (relevant for carbonation and chloride penetration), but their increased porosity
lower freeze–thaw resistance. Cement-based mixes offer a sustainable solution for this waste in applications with
moderate or non-structural requirements.

1. Introduction
The mining of primary natural resources generates a large amount of
waste, which has a sizable physical footprint and, in some cases (such as
for sulphidic tailings), poses a serious threat to the surrounding envi­
ronment. For those tailings where there is a threat, specialized storage is
needed. Finding new uses for tailings is one of the most important steps
toward making the mining industry more sustainable. Due to their high
production volume (roughly 700 Mton per year in Europe [1]), tailings
can be used as a substitute for natural aggregates. Furthermore, the
amount of tailings is expected to grow over the next decades as ore
grades continue to decline and metal demand is forecast to rise
dramatically [2]. The massive volumes of mining waste generated make
its full utilization a challenge for the circular economy strategy.
Although the use of cemented paste backfills (consisting of 3–10 wt%
Portland cement) has proven to be a fruitful valorization strategy [3],
other, potentially more lucrative options, should be investigated. Mul­
tiple strategies must be employed for the effective management of the
various waste streams, and given the recommendation of maximizing
value retention [4,5], special emphasis must be put on the prospect of
upcycling.
However, due to their fineness, mine tailings cannot be used as an
aggregate in cement-based materials. An alternative recycling of mine
tailings as aggregates employs cold granulation techniques. This strat­
egy has been used effectively to create artificial aggregates mainly from
other fine materials like fly ash [6–8]. Specific considerations are needed
when producing cold-bonded artificial aggregates from mine tailings (e.
g. limited contribution to microstructure development, presence of
minor elements, water demand), potentially leading to a significant
demand for binder for the application [9].
The manufacturing of artificial granules from sulphidic mine tailings
using cold granulation with cement has been optimized in previous
studies [10]. The usage of 5 % CEMIII/B (and 95 % tailings) allowed the
production of aggregates suitable for cement-based products. That
similar cement contents as those used in backfilling applications may
combine with uses of the material in substantially higher value appli­
cations is quite promising. Initial research into the use of these granules
in mortar mixes has been auspicious, revealing efficient leaching control
of heavy metals and compressive strength values of 44 MPa when uti­
lizing up to 32 wt% of granules in relation to the total sand content in
mortars using a CEM III/B binder [10]. The strength level was main­
tained even with such content of granules in comparison with mortars
made with only siliceous sand. This is also a higher value than the one
reported by other researchers [11–13], who observed values around 30
MPa for similar applied ratios of cold-bonded granules. The results in [8]
seem more advantageous as above 50 MPa were still achieved with a
ratio content of cold-bonded aggregates of 50 vol%. Irrespective of the
type of cold-bonded aggregate, as its volume in concrete increases, its
compressive strength decreases. However, the primary affectation by
the porosity of granules occurred in the fresh state. Workability is
drastically reduced due to the high water absorption capacity of the
artificial granules; hence, further mix optimization is required. Despite

* Corresponding authors.
E-mail addresses: yury.villagranzaccardi@vito.be (Y. Villagran-Zaccardi), arne.peys@vito.be (A. Peys).

https://doi.org/10.1016/j.conbuildmat.2023.134049
Received 17 July 2023; Received in revised form 28 September 2023; Accepted 1 November 2023
Available online 9 November 2023
0950-0618/© 2023 Elsevier Ltd. All rights reserved.
Y. Villagran-Zaccardi et al.
the fact that the high water absorption capacity limits the usage of cold-
bonded aggregates in concrete, scarce literature suggests the use of
appropriate dosages and types of superplasticizers to eliminate this
drawback [14].
As a porous constituent, it is also expected that the inclusion of cold-
bonded aggregates will result in reduced durability performance.
Transport properties are important factors related to durability perfor­
mance. In general terms, an increase in transport rate means a reduction
in durability performance. However, there are some important excep­
tions. Carbonation and chloride penetration depend on both the trans­
port rate into concrete and the binding capacity of the matrix. Cold-
bonded aggregates are composed of small amounts of cement, and the
corresponding hydrates would provide additional binding capacity, i.e.,
buffer capacity for carbonation or chloride ingress. Thus, the correlation
between porosity and durability performance would be attenuated in
this regard.
Therefore, the purpose of the present research is to conduct a more
in-depth analysis of how superplasticizers can be used to enhance
workability, strength, and durability performances of mortar and con­
crete mixes. Mechanical performance is generally addressed in the
literature, but strategies to counteract the effects of artificial granules on
workability or durability performance are lacking. Mortar and concrete
samples with 17 and 32 wt% of granules replacing natural aggregates
were produced. Mortar samples were tested for flow at 5 and 30 min
post-mixing and for compressive strength and porosity using prisms also
cast 5 and 30 min post-mixing. Concrete samples were tested for slump,
air content, compressive strength, carbonation rate, chloride migration,
and frost scaling resistance.
2. Materials and methods
The Boliden processing facility was the source of the mine tailings
(Tara, Ireland). The coarse fraction is used at the mine site to create
backfill, so only the fine fraction from the tailing pond was utilized for
this research. The tailings were sourced from the Tara tailings storage
facility (TSF) using an experimentally supported excavation strategy to
obtain a sample of 25 tons of tailings that is representative for the cur­
rent production in terms of particle size and phase composition. Samples
from 14 locations around the TSF were taken for analysis and 1 location
was selected. Drilling cores enabled the generation of a depth profile.
Based on this data, the material was excavated from the south side of the
TSF, scraping only the top 1 m of the slurry. The material was pre-dried
in the sun and completely freed from moisture using flash drying at
thyssenkrupp.
The chemical and mineralogical compositions of tailings and CEM
III/B are displayed in Table 1. Mine tailings had a D10/50/90 of 1.7/
8.3/33.7 µm, while cement had a D10/50/90 of 1.8/10.0/26.0 µm.
The granules were produced using an upscaled version of the pro­
cedure in previous work [10]. At a ratio of 6 wt% CEM III/B 42.5 N and
94 wt% mine tailings, granules were generated in an Eirich R08W high-
intensity mixer for solids. This cement content in this methodology is
considerably lower compared to those reported in similar strategies for
producing cold-bonded lightweight aggregates (e.g. 10 wt% as
mentioned in [15;16]). This substantial decrease in cement usage pro­
motes environmental sustainability and offers a more competitive pro­
duction cost. The granules were made by first thoroughly combining the
dry ingredients, and then gradually adding 8 L of water for 50 kg of dry
Table 1
Chemical compositions (XRF) of mine tailings and cement, and mineralogical composition (XRD + Rietveld analysis, see Supplementary Material) of tailings.
wt.% CaO SiO2 SO3 MgO
CEM III/B 49.5 29.8 3.2 5.9
Tailings 27.6 28.2 3.0 3.2
wt.% Calcite Quartz Dolomite Muscovite/illite
Tailings 47.3 20.9 15.7 6.7
2
Construction and Building Materials 409 (2023) 134049
ingredients. To generate microgranules, the water and powders were
mixed at high rotor speed (1500 rpm) and low pan speed (25 rpm), and
then the rotor was set at lower speed (250 rpm) and the pan was set at
higher speed (50 rpm) to facilitate granule growth. The total production
of granules was 1.2 ton, which was achieved in 3 shifts of 6–8 h.
Granules with two size ranges were produced by controlling the time
of this last granule growth stage, one with a nominal size of 1–4 mm
(Fig. 1) for sand replacement, and one with a nominal size of 2–8 mm for
aggregate replacement. The particle size distributions of the granules
1–4 and 2–8 mm are presented in Fig. 2. The water absorption and dry
density of the 1–4 and 2–8 granules produced were 7.6 and 8.5 %, and
1.58 and 1.48, respectively. This value places them in the lowest range
of water absorption capacities (4.7–28.8 %) reported in the literature for
similar cold-bonded artificial aggregates [17]. Whereas the composition
of the pilot produced granules was very similar to the lab granulated
counterparts [10], the water absorption values were very much
improved (8 % versus 13–16 %). The microstructure of the pilot gran­
ules handled in the present paper shown in Fig. 1 reveals a larger pore in
the centre of the granule with a dense shell, which was not observed in
the lab granules. The higher energy and centrifugal force provided by
the larger mixer has densified the outer part of the granules, rendering
the water to be less easily absorbed, despite the lower density of the
granule. However, even the lab granules provided water absorption
values in the lower range of relevant literature. The limited amount of
cement used incorporated small amounts of C-S-H in the granules, which
had a very limited impact on the water uptake of the particles.
The optimized granules were used as aggregate in mortar and con­
crete mixes. The mortars were optimized for maintaining the consis­
tency level and checking the flow loss over time. In addition, effects on
compressive strength and porosity were verified. Concrete mixes were
designed based on observations of the performance of mortars in the
fresh state, and their performance in terms of strength and durability
was assessed.
For the mortars, aggregate packages were prepared by replacing 17
wt% and 32 wt% of standard CEN sand with 1–4 mm granules. The
replacement ratios were decided on the basis of results in previous work
[10]. In order to preserve a similar distribution of particle sizes, the CEN
sand was replaced so that half or all of the 1- to 2-mm particles were
replaced (17 and 32 wt% overall replacement ratios, respectively). For
the sake of comparison, a control mixture was also made with 100 %
CEN sand. The compositions had a 3:1 mass ratio of aggregate to cement
and a 0.5:1 mass ratio of water to cement. The mixing was performed in
accordance with EN 196–1, using a Hobart mixer. The consistency of the
mortar mixes was assessed on a flow table in accordance with EN
1015–3 after mixing was complete (approximately 5 min following the
addition of water in mixing), and again 30 min after the start of mixing
to check the consistency loss. Before the second flow measurement, the
mortar was remixed at high speed for 60 s. After each consistency test,
specimens were cast to evaluate the material’s performance in the
hardened state. All casting, compaction, and curing processes (in clim­
atized room) adhered to the procedures outlined in EN 196–1.
As shown in Table 2, several mortar mixes were made by adding
water and/or superplasticizer to approximate the desired consistency
level (i.e., a value comparable to that of the REF mix). Master Glenium
51 (35 wt% solid residue) was used as the superplasticizer (SP). The SP is
expressed as the % of solid SP relative to cement. In the case of G17A and
G32A, proportions were corrected by adding 70 % of the water
Al2O3 Fe2O3 BaO Others
8.5 1.4 / 1.7
5.2 2.3 2.0 3.3
Microcline Albite Baryte Pyrite
2.3 2.9 2.4 1.8
Y. Villagran-Zaccardi et al. Construction and Building Materials 409 (2023) 134049

Fig. 1. Produced granules (size < 4 mm). Left: external appearance; right: microstructure under SEM.

combination of the previous two approaches was used, resulting in an

intermediate reduction of the effective water-to-cement ratio compared
to the previous cases while also increasing robustness. After 28 days of
curing, compressive strength and porosity from water absorption upon
vacuum saturation of mortar samples were determined.
Concrete mixes were also prepared with proportions as reported in
Table 3. A reference mix with natural aggregates was used for com­
parison purposes in the assessment of concrete mixes containing 17 wt%
and 32 wt% of granules replacing both fine and coarse natural aggre­
gates, M17 and M32, respectively. The slump, unit weight, and air
content (pressure method) were determined according to EN 12350–2
and 12350–7, respectively. The coarse capillary porosity and total
accessible porosity were determined upon water saturation under vac­
uum. For the saturation, samples were first placed in a chamber under
vacuum (<0.05 bar) for two hours; then, tap water was introduced in the
chamber without releasing the vacuum until the samples were covered
(~25 mm). The vacuum was maintained for only 1 additional hour.
Samples were maintained under water until they completed a 24-h
Fig. 2. Particle size distributions of produced granules 1–4 mm and 2–8 mm.
period. To compute the coarse capillary porosity, samples were dried
at (40 ± 2) ◦ C for 7 days, and the weight loss during this drying was
Table 2 compared to the total volume of samples. For the total accessible
Mortar mixes with consistency optimization. porosity, samples were further dried at (105 ± 5) ◦ C for 48 h, and the
weight loss relative to the saturated state was compared to the total
Granules content ID Correction strategy for achieving target consistency
(wt.%)
volume of samples.
The use of waste materials in building items requires the evaluation
0 REF None
of the environmental quality of such an application. Batch leaching
17 G17 None
G17A Addition of 70 % of water absorption capacity of experiments provide the potential release of elements of interest. The
granules hardened mortar and concrete mixes leachates were investigated
G17B Addition of 0.06 wt% of SP following the methodology as described in EN 12457–4. First, samples
G17C Addition of 0.10 wt% of SP
coming from the remaining material after the compression tests were
32 G32 None
G32A Addition 70 % of water absorption capacity of
granules
G32B Addition of 0.10 wt% of SP Table 3
G32C Addition of 0.16 wt% of SP Proportions and properties of concrete mixes.
G32D Addition of 50 % of water absorption capacity of Materials Amounts (kg/m3)
granules and 0.11 wt% of SP ID M0 M17 M32

River sand 792 616 467

absorption capacity of the granules to achieve the target consistency Crushed limestone 6–14 967 752 570
Granules 1–4 126 220
level. This approach is based on the assumption that only a fraction of
–
Granules 2–8 – 154 268
the water absorption capacity of highly absorbent aggregates is effec­ CEM III/B 42.5 N 355 355 355
tively saturated by water uptake of the dry particles incorporated in the Water 177 178 178
fresh mix [18]. Under this premise, the effective water-to-cement ratio Additional water 5 16 25
Superplasticizer 0.2 0.5 1.3
remains unaffected even though granule particles are actually not fully
Properties
saturated within the fresh state. For G17B, G17Cm G32B, and G32C, the Air content (%) 2.6 3.1 3.8
consistency level was procured with the aid of SP in variable contents. Slump (mm) 100 100 150
As a result, the effective water-to-cement ratio in these mixes was Unit weight (kg/m3) 2368 2309 2274
reduced as dry granules absorbed water from the fresh matrix, but the SP Total accessible porosity (%) 16.0 19.1 21.8
Coarse capillary porosity (%) 6.5 7.6 9.1
prevents that this reflects on the workability of the mixes. For G32D, a
Compressive strength, 28d (MPa) 45.3 ± 2.2 38.8 ± 0.5 35.5 ± 1.3

3
Y. Villagran-Zaccardi et al.
prepared by crushing them mechanically to a particle size of < 4 mm.
Representative subsamples were taken from each crushed material, and
the moisture content was determined. Preparations of 1:10 solid:water
ratios were made, with extraction times of 24 h on a shaking table. The
liquid phase was later filtered (45 µm membrane), and measurements
were performed on the liquid for pH and ICP analysis for As, Pb, Cd, Cr,
Cu, Ni, Zn, Sb, Ba, Mo, V, Co, Se, Sn, and sulfate.
To better describe the microstructure of the mortar containing
granules, fluorescent microscopy on thin sections was applied. The
studied samples were from mortars G32, G32A, and G32D, both cast
immediately after mixing (G32x-0) and cast 30 min after the end of
mixing (G32x-30). The hardened mortar samples already cured for 28
days were impregnated with fluorescent epoxy and polished to prepare
thin sections. Ten images of the granules in each thin section were ac­
quired using transmitting light and the UV filter at a magnification of
20X. Locations were random but focus was made on the developed
interfacial transition zone (ITZ) between granules and the matrix. The
thickness of the ITZ at four points in each image was measured.
The carbonation resistance was measured in two prisms with di­
mensions of 100 x 100 x 400 mm3 per mixture in accordance with NBN
EN 13295. The specimens were cast and cured in a room at RH > 95 %
and 20 ◦ C until the age of 28 days. After that, conditioning continued by
placing them in a controlled environment at 20 ◦ C and 60 % RH for 14
days. Initial measurements were made before exposure in the carbon­
ation chamber, and the specimens were then stored in a controlled
carbonation chamber with a concentration of 1 % CO2, temperature of
20 ◦ C and RH 60 %. Subsequently, the measurements of the carbonation
depth were done after exposure periods of 7, 28, and 56 days. Each time,
the prisms were split at about 50 mm from one end, and one freshly
broken surface was sprayed with phenolphthalein. The remaining parts
of the specimens were further stored in the carbonation chamber until
the next measurement. The depth of the revealed carbonation front was
measured at 5 points for each side of the sprayed surface, to determine
average values and standard deviation.
In addition, chloride migration coefficients were measured for each
concrete mix. Cylinders with a diameter of 100 mm were first cast and
Table 4
Consistency of fresh mortar mixes.
4
Construction and Building Materials 409 (2023) 134049
cured for 28 days at 20 ◦ C and RH > 95 %. A disc of 50-mm thickness
was sawn out of the centre of each cylinder and preconditioned for the
testing. The samples were first put under vacuum for 3 h, and saturated
Ca(OH)2 solution was then added to cover up the samples while main­
taining the vacuum for another hour. The vacuum was finally released to
produce the full saturation of the samples, which were maintained under
solution for additional (18 ± 2) hours. The test specimens were isolated
with rubber sleeves, which also served as containers for the anolyte. The
samples in the sleeves were placed in a container with 12 L of 10 % NaCl
solution as catholyte. Inside the rubber sleeves, 300 ml of 0.3 M NaOH as
the anolyte solution were added. The cathodes and the anodes were
connected to the power supply, and the current was adjusted as indi­
cated in NT Build 492. After the prescribed test duration of 24 h, the
specimens were removed from the device, rinsed, and axially split. The
freshly broken surface was sprayed with a 0.1 M silver nitrate solution to
reveal the chloride penetration front. This chloride penetration was
measured at 7 locations, and used for computing the chloride migration
coefficients as indicated in NT Build 492.
Concrete specimens were also tested for freeze–thaw scaling resis­
tance in accordance with Technical Specification CEN/TS
12390–9:2016, alternative method “Cube test”. In this method, 100-mm
cube specimens are subjected to freeze–thaw while immersed in a 3 %
sodium chloride (NaCl) solution. The mass loss of the cubes for up to 56
freeze–thaw cycles was used to assess the freeze–thaw resistance.
3. Results and discussion
3.1. Fresh properties
Table 4 displays the mortar’s consistency after 30 min. Fig. 3 displays
the corresponding flow values, including both the initial value and the
consistency loss 30 min after mixing began. Both the G17C and G32D
mixtures achieve the target flow values, immediately after finishing
mixing and after 30 min, respectively. The lack of fluidity displayed by
Mixes A is indicative of the limitations of the sole addition of extra water
to compensate for the granules’ water absorption.
Y. Villagran-Zaccardi et al.
Fig. 3. Flow values for mortar mixes.
The results for the concrete mixes (i.e., slump values in Table 3)
demonstrated that small adjustments of the superplasticiser content
were sufficient for compensating the affectation of workability by the
porosity of the granules.
The demand for additional superplasticizer suggests an increase in
the production costs for these mixes. However, the cost of a concrete mix
can be affected by several factors, and the amount of superplasticizer
used is only one of them. Superplasticizers can help reduce the amount
of cement needed to produce a given volume of concrete; this is espe­
cially true for mixes with low strength requirements [19]. Even though
superplasticizers are typically more expensive than other concrete in­
gredients such as cement, sand, and aggregate, the cost of a super­
plasticizer can also be variable depending on type and quality. Factors
such as the location, the size of the project, and the complexity of the
mix design can also affect the cost of a concrete mix to a greater extent
than the amount of superplasticizer.
3.2. Compressive strength and porosity
Fig. 4 displays the results of compressive strength of mortar mixes.
By comparing the results of samples cast immediately after mixing to
those cast 30 min after mixing, we see that the compressive strength of
granule-containing mortars increases slightly. From the individual
comparisons between samples cast immediately after mixing and sam­
ples cast with 30 min delay, in most of cases the difference between
average values surpasses the sum of the standard deviations for the
Fig. 4. Compressive strength versus porosity (from water absorption under
vacuum) of mortar samples at 28 days (average ± standard deviation) (see the
Supplementary Material for more details on the data in the graph).
5
Construction and Building Materials 409 (2023) 134049
respective series, demonstrating that these differences are statistically
significant. Overall, the average increases are 2.179 and 3.41 MPa for
mixes with 17 and 32 % granules, respectively, with respective 95 %
confidence intervals of [0.04–4.32] and [0.62–6.20] MPa. A corre­
sponding inverse trend is presented by the porosity results, with statis­
tically significant (95 % confidence intervals) reductions of the average
porosity of 0.93 [0.12–1.74] and 1.71 [-0.10–3.52] percentage points
resulting from the values presented in Fig. 4. A similar trend is observed
for the reference mortar, but to a much-reduced extent than the samples
containing granules. Further detail of the data presented in Fig. 4 can be
found in the Supplementary Material.
Standard compaction is quite vigorous (60 jolts for each of the two
layers), and this guarantees good compaction levels for all these com­
binations, as all of them were sufficiently cohesive, even though they
were not always showing adequate workability. Then, the influence of
the granules within the first 30 min explains the discrepancy in
compressive strength, rather than the compaction degrees themselves.
Granules were employed unsaturated, so as soon as they came in contact
with the mixing water, they began to absorb part of it. The water-to-
binder ratio of the matrix decreases when this fraction of water is
absorbed (particularly in the first 10 min [20]). This water absorption
would influence the immediate layer of matrix covering each granule
particle and establish a water-to-cement gradient when the samples are
already cast soon after mixing. After 30 min, the gradient will be gone as
water absorption mostly occurs before the re-mixing (i.e. the mortar mix
is homogenised). Remaining water uptake after 30 min is low, and the
final matrix seems more homogeneous (see further microstructural an­
alyses in section 3.4). The second scenario is more similar to common
production practices because 30 min is a normal amount of time to
manipulate the mix. It is expected that in practice there would be a more
significant impact of the workability of the mix on the compression
strength, as the compaction energy is lower than the applied standard
procedure. Since consistency optimization fixes workability problems,
the relationship between workability and compressive strength becomes
of secondary importance. Then, blends G17C and G32D emerge as the
most promising candidates for large-scale use in concrete (i.e., similar
consistency level and loss to that of REF mix).
Thus, the porosity of granules tends to lower the compressive
strength of mortar, but the effect is more complex than just the one from
the volume of these granules. Compressive strength level can be uphold
once consistency and water content are decoupled. In the mortar mixes,
no significant effects of the interfacial transition zone on the compres­
sive strength are noticed. The sole improvement of the matrix is suffi­
cient for the compressive strength level under analysis. The mortar
Y. Villagran-Zaccardi et al. Construction and Building Materials 409 (2023) 134049

mixes with granules remain more porous than the reference mix, but
they are able to reach similar compressive strength levels. Unsaturated
granules absorb water in the mix and reduce the water-to-binder ratio up
to a certain extent. Such a reduction of the water-to-binder ratio appears
sufficient to maintain the compressive strength at 17 % granule content.
This means that water absorption in fresh G17C somewhat compensates
for the higher porosity of the granule particles when given enough time
to occur and the remixing is applied after 30 min. However, for the
workability of G32D to be maintained at the same level as that of the
reference mix, the necessary water and superplasticizer addition inevi­
tably decreased the compressive strength of the mortar even when
remixing after 30 min. This was the case because only up to a certain
degree of fluidity loss may be addressed by using a superplasticizer with
32 % granule content. Complete compensation with superplasticizer still
resulted in substantial flow loss over time in G32C, so the use of
superplasticizer had to be complemented with some additional water to
achieve and maintain the target workability in G32D.
The mortar matrix still contains the granules as a porous phase.
Therefore, regardless of the granule content, all mortar mixes share a
similar relationship between porosity and compressive strength Fig. 4.
Similar to other studies in the literature [21–23], the crushing strength
of the granules governs the compressive strength of mortar and concrete.
For the concrete mixes, the presence of the porous granules leads to a
reduction in the compressive strength, but the situation is different for
the mortar mixes. The crushing strength of aggregates might be critical
for high compressive strength levels. However, for the designed mixes
and granule contents, the microstructure of the granules was not critical
for the mechanical performance of mortars. By modifying the consis­
tency with the superplasticizer, we were able to keep the mix at a similar
consistency and compressive strength to that of the reference mortar
when granule content was 17 %. It is important to say that the whole
strategy involves the same cement demand as current practices. First,
the cement content used for the production of granules is equivalent to
that currently used in backfilling. Second, for 17 wt% granule content,
the total cement content for achieving the equivalent compressive
strength of the reference mortar mix was the same. A Life Cycle
Assessment of the processing and application in mixes as a whole is still
needed to quantify the benefits of this valorisation technique.
content. The use of synthetic aggregates increases Pb leaching, but this is
still within the limits. No strong correlation between the Pb release and
the granule content was detected. The values are slightly lower than
those previously reported when using the same CEM III/B and 32 %
granules [10], and they are in agreement with an enhanced encapsu­
lating capacity provided by high blast furnace slag concentrations in the
cement [24]. Cu and Zn leaching was also detected, but at values far
below the limits. The element demonstrating the highest presence in the
leachate was Ba, but as mixes containing 32 % granules showed lower
values than those containing 17 % granules, this is attributed more to
the cement than to the granules. Overall, the heavy metal encapsulation
capacity in the cement-bound granules is well sustained and more
favourable than similar approaches in the literature [25,26], especially
for the encapsulation of Cu. Despite no leaching tests were conducted
regarding the potential for secondary use of the concrete mixes, the
diminished concentration of granules correspondingly decreases the
leaching rate from crushed concrete compared to crushed mortar to an
extent that renders such tests redundant. Therefore, the compliance for
the mortar mixes is extensive to the concrete mixes. It should be noticed
that these results are valid for particular tailings used in this study and
may not represent other more challenging tailings with higher contents
of heavy metals.
The mechanism through which the heavy metals are bound in the
material is connected with the presence in the granules of hydration
products from the cement containing ground granulated blast furnace
slag (CEM III/B). This has been confirmed in previous studies [10,29]
and explained by the significant role of calcium silicate hydrates (C-S-
H). Absorbability, low permeability, inhibiting liquid migration, and the
presence of gel pores are all important aspects defining the strong
immobilization actions of C–S–H [30]. The inclusion of ground granu­
lated blast furnace slag contributes further with additional calcium
aluminate and sulfoaluminate hydrates. Calcium sulfoaluminates (e.g.
ettringite) can incorporate mono- and bi-valent cations and anions and
also form solid solutions with heavy metals (e.g., Cr, Mo) [31]. There­
fore, the benefits of CEM III/B are not restricted to the cold granulation;
it also improves the environmental quality of the granules.
3.4. Microstructure by fluorescent microscopy

3.3. Leaching An example of fluorescent microscopy is shown in Fig. 5 (the rest of

the images can be found as Supplementary Material). A particle of the
Tests were performed on crushed mortar samples following the 28- granulate can be seen with variable porosity between the different
day compressive strength tests and are presented in Table 5. Only component phases. Some tailing particles with very low porosity (e.g.,
meaningful values are presented, whereas determinations for As, Cd, Co,
Cr, Mo, Ni, Sb, Se, Sn, and V, in all these samples were under detection
limits. The crushed mortar leftovers from the 28-day compressive
strength tests were used in the leaching test to check compliance with
the limit values for the second life valorization such as use in unbound
applications. Duplicate determinations were made on G17A, G17C,
G32A, and G32D, as references and best candidates for superplasticizer

Table 5
Duplicate batch leaching results of the mortars incorporating synthetic aggre­
gates replacing sand, compared to the VLAREMA B2.3.2 limits for use in con­
struction materials [27] and the EU inert waste legislation limits [28]. Elements
for which no limits are defined are indicated with a “/”.
mg/ G17A G17C G32A G32D VLAREMA EU Inert
kg limit waste limit

Pb 0.27/ 0.28/ 0.33/ 0.34/ 1.3 0.5

0.28 0.31 0.32 0.32
Cu 0.06/ 0.07/ 0.11/ 0.10/ 0.5 2
0.11 0.10 0.10 0.10
Zn 0.15/ 0.17/ 0.16/ 0.19/ 2.8 4
0.19 0.19 0.19 0.21
Ba 14.00/ 13.00/ 8.20/ 8.30/ / 20
Fig. 5. Example of fluorescent microscopy and measurement of the interfacial
12.00 14.00 7.70 8.00
transition zone thickness between granules and new matrix.

6
Y. Villagran-Zaccardi et al. Construction and Building Materials 409 (2023) 134049

quartz) show a variable size, varying from less than 1 μm to a few tens of
μm. Some of these particles are located outside the transition halo. This
is indicative of some attrition of the granules during mixing, which were
releasing part of their mass into the new cement matrix. Alternative
explanations for these particles, such as unreacted slag particles coming
from the cement, should not be discarded because these are depicted in
the SEM images (Fig. 1, left). The perimeter halo depicts the ITZ. This
zone develops with variable thickness for the different mortars.
To determine the thicknesses of the interfacial transition zone, four
ITZ thickness measurements were made for each of the 10 images taken
per type of mortar. These measurements were located randomly,
avoiding the areas affected by interaggregate distance, in an effort to
isolate as much as possible the individual effect of the granules. Box
plots for the interfacial transition zone thicknesses are shown in Fig. 6.
The images and measured values can be found in the Supplementary
Material. The values are slightly larger than those typically reported for Fig. 7. Accelerated carbonation of concrete mixes.
natural aggregates in hardened concrete (10–50 μm) [32,33]. No sig­
nificant differences are noted between the different mortars. This is interpreted as the result of a dual effect of granules in the mix. On the
expected since there are no major differences in the composition of the one hand, granules act as porous particles embedded in the matrix and
mortars. The main difference between the G32, G32A, and G32D series offer a preferential path for all transport processes, including CO2
is that the first one has no water compensation for aggregate absorption, diffusion. On the other hand, granules contain a certain amount of
the second one has water compensation, and the third one has a small cement (about 8 wt%), and the corresponding hydration products are
compensation for mixing water and a contribution to workability with able to provide additional alkaline reserve to bind more CO2. It should
the use of the superplasticizer. Thus, the interfacial transition zone be mentioned that most of the granules did not show significant alka­
would have been affected differently depending on the amount of water linity during the colorimetric tests (see for example Fig. 8, which shows
absorbed by the granules in the fresh mortar. There is a small tendency little to no coloration of the granules when sprayed with the phenol­
to show a slightly thinner interfacial transition zone for mortars cast 30 phthalein solution). Thus, such a contribution in terms of binding ca­
min after the start of mixing compared to mortars cast immediately after pacity would not be extremely high. This is most probably due to the low
the end of mixing. These 30 min would have allowed sufficient time for amount (6 wt% of the total dry matter) and type (CEM III/B) used for the
water to be absorbed, and remixing prior to casting would have resha­ manufacture of the granules. Other authors [35] have reported signifi­
ped the interfacial zone. The cement paste penetration into the surface cant alteration of the C-S-H microstructure when subjecting cement-
pores of the unsaturated granules results in mechanical interlocking bonded granules to high CO2 curing conditions. Despite the quite vari­
between the granule particles and the cement matrix, resulting in a able situation that is to be expected depending on the natural carbon­
good-quality ITZ [34]. Since the granules do not interact with the matrix ation degree that granules experience during storage, the granules used
with the same intensity as in the immediately cast mortars, the interface in the present study were not fully carbonated at the moment they were
gradient develops at a lower thickness. used (revealed by the slight coloration of the granules after they
spraying with phenolphthalein, Fig. 8). This confirms that the micro­
structure of C-S-H in the granules was not altered, and that the granules
3.5. Carbonation
designed were therefore sufficiently stable under natural storage. The
main parameters in terms of carbonation would be the particle size of
The results from the accelerated carbonation tests are presented in
the granules and their age. The dual effect of providing alkaline reserve
Fig. 7. There is a certain variation of results within the expected range
and porosity couples with the additional physical effect of supplemen­
for the type of experiment. Even though the trend indicates faster
tation of the particle size distribution of the granular skeleton. Overall,
carbonation for 17 wt% of granulate content, the lack of correlation
the balance of the multiple effects resulted in a maximum increase of 20
between carbonation rate and granule content of mixes can be

Fig. 6. Interfacial transition zone thickness between granules and new matrix.

7
Y. Villagran-Zaccardi et al. Construction and Building Materials 409 (2023) 134049

Fig. 8. Colorimetric test of M32 sample at exposure time = 0 d.

% in the carbonation rate for M17 compared to M0 as a reference. Using

32 wt% of granules decreased the carbonation rate with respect to M17,
and reflects almost the same carbonation rate as the reference mix. This
highlights the contribution of the buffer capacity of the granules in terms
of carbonation.
These results originate from the accelerated protocol for the test,
with a CO2 concentration of 1 %, RH = 60 %, and temperature of 21 ◦ C.
Under natural conditions the situation may be somehow different.
Especially in concrete elements subjected to weathering, it is expected
that the wetting and drying cycles will play a significant role in the
carbonation process [36]. In this sense, the changes in pore structure
associated with the use of granules would affect the absorption and
drying rates of the concrete. The more porous granules may act as res­
ervoirs of moisture embedded in the drying cement matrix. These would
absorb additional water during wetting and delay the drying process
afterwards. It seems difficult to predict how such an effect would change
the overall impact of the granules on the resistance against carbonation
of the concrete, and further research would be valuable for confirmation
of the expected service life of this type of concrete.
The impact of the granules on the carbonation performance is much
lower than the one that can be expected from the analysis of the porosity
and compressive strength of the concrete mixes. The cement hydrates
contained in the granules clearly consumes carbon dioxide and mitigates Fig. 9. Chloride penetration profiles after chloride migration experiment.
further penetration of the carbonation front. Cement-bound artificial
aggregates contribute to the buffering capacity of concrete.
Table 6
Average and [95% confidence interval] of chloride migration coefficients.
3.6. Chloride migration Series Non-Steady migration coefficients [10-12 m2/s]

Fig. 9 shows the chloride penetration profiles in the concretes with
the different granule contents. The concretes containing granules have a
higher porosity, but this did not translate directly to greater chloride
penetration. Among the series, the average chloride penetration is
similar, leading to similar chloride migration coefficients, as shown by
the calculations in Table 6, where no statistically significant difference
between the series is observed. All values correspond to the range of
high resistance to chloride penetration [37]. A certain trend of small
increments in the value of the chloride migration coefficient may be
considered. However, with 17 % and 32 % granules, profiles with
greater variability are noted. This may be associated with the higher
porosity of granules combined with their limited cement content. When
95 % confidence intervals are considered, no significant difference
M0 5.00 [4.64–5.36]
M17 5.35 [4.97–5.72]
M32 5.42 [4.65–6.19]
among series is noted. Regarding chloride penetration, cement hydrates
are able to contribute greatly by binding chloride [38], and this amount
of chloride is not free anymore to continue penetrating in depth. Chlo­
ride binding is a delaying process during chloride penetration. Thus, the
location of the granules plays a dual role: on the one hand, it provides
localized porosity in the concrete volume that enhances chloride pene­
tration, but on the other hand, it also provides chloride retention ca­
pacity (as a function of its cement content) that delays chloride
penetration. The result is then that the higher porosity is partially

8
Y. Villagran-Zaccardi et al.
compensated by the chemical activity of the granules in terms of chlo­
ride ingress.
Chloride migration experiments cannot address some aspects of
chloride penetration in reinforced concrete structures in service. The
experiment is conducted in saturated state, and for those structures that
are not permanently under water the transport process differs slightly.
The macroporosity normally does not take part in the chloride pene­
tration in atmospheric exposure [39], as these pores are never saturated
unless the structure is under water. A portion of porosity incorporated in
the concrete mixes by the granules is coarse capillary porosity (which
can be emptied from moisture when drying at 40 ◦ C). The coarse
capillary porosity that can be attributed to the inclusion of the granules
(differences between values for M17 and M32 series with respect to M0
in Table 3) represents 5.8 % and 11.9 % of the total porosity in M17 and
M32, respectively. Such values may not be very big figures, but these
still suggest that differences in the resistance to chloride penetration due
to the inclusion of granules would be less than the differences depicted
in Table 6 for concrete exposed under unsaturated conditions. In terms
of application, it can be expected than concrete containing these gran­
ules will perform even better in realistic conditions than reported here.
Similar to the results from carbonation, the impact of the granules on
the chloride migration coefficients is very low. Again, the buffering
capacity provided by the cement hydrates contained in the granules
compensates for the more porous microstructure. In the case of chloride
migration this buffering effect is enhanced by the use of CEM III/B in the
production of the granules, as ground granulated blast-furnace slag is
well known for its high chloride binding capacity [40].
3.7. Freeze-thaw scaling
Among the applied durability assessments, probably the most
demanding attack was the frost-scaling test (Fig. 10). The weight loss
after 56 cycles shows an inverse proportionality with the compressive
strength of the concrete mixes at 28 days. The physical attack during the
freeze–thaw cycles is associated with the porosity of the concrete mix to
a similar extent as the compressive strength. The casting of samples
inherently generates a cement skin with higher porosity and lower
strength due to the wall effect against the moulds. This is due to the
effect caused by the cement paste at the surface of concrete (1–2 mm)
where aggregates are less present. This weaker surface layer is exposed
and lost first during the scaling test. A big proportion of the difference
among the mixes is due to the weight loss during the first 7 cycles,
meaning quite different quality of the concrete skin due to the presence
of granules. After the initial loss of the cement skin, the interpretation of
the progression of the weight loss over time seems more intuitive, as the
presence of the porous granules in the bulk would also speed up the
deterioration process. Given the porosity of the granule particles, for the
analysis of frost-scaling and strength, it seems more convenient to
Fig. 10. Weight loss due to freeze–thaw-scaling.
9
Construction and Building Materials 409 (2023) 134049
address these particles as weaker spots within the matrix, rather than
“aggregate” particles. It is clear that the microstructure of the granules is
more comparable to that of the cement matrix than to that of natural
aggregates. As such, they would become part of the skin of the concrete
when next to the surface and translate into a slightly increase in the
cement skin thickness (Fig. 11). Contrary to virgin aggregate particles,
the granules would increase the thickness of the concrete skin rather
than reduce it. The same applies for the content of paste in the bulk of
the hardened concrete. The results of the frost-scaling test can therefore
be explained straightforwardly by the relative volume of porous phase
(matrix + granules) at the surface and in the bulk of the concrete.
4. Conclusions
Artificial granules were made to study a potential valorisation route
for sulfidic tailings from a lead–zinc mine. The granules were produced
at pilot scale using 6 wt% CEM III/B as binder (94 wt% of tailings). The
resultant hardened cement-bound aggregates were tested for application
in mortars and concrete. Optimization of consistency in mortar mixes
was effective and had no negative impact on strength or porosity when
small replacement levels are used. Superplasticizer effectively reduced
workability loss for a content of granules of 17 wt% without the loss of
compressive strength. A content of 32 wt% of granules did result in a
slightly decreased strength in samples with optimized consistency, as a
combination of 50 % of the water absorption capacity of the granules
and superplasticizer was necessary. Overall, the technical feasibility of
the mixes was demonstrated. The granules keep their porous nature
when in the mortar matrix. There is no difference in the relationship
between porosity and compressive strength across different mortar
mixes with variable granule contents (i.e., all mortar mixes fall into a
single linear relationship between porosity and compressive strength).
The results from leaching of heavy metals demonstrated no partic­
ular concerns regarding the second life application of mortar and con­
crete made with these granules. It seems that exclusively from this point
of view there is margin to increase granule contents even above 32 %.
The durability performance of concrete that incorporates these
granules is determined by an interplay between physical effects derived
from the intrinsic porosity of the granules and chemical effects attrib­
utable to their content of cement hydrates. The penetration of CO2 and
chloride is promoted by a more interconnected porosity with increasing
granule content, which seems in turn counterbalanced by an increased
buffering capacity.
For carbonation, the influence of the porosity is found to be pre­
dominant for the 17 % of granule content, leading to faster carbonation,
and more balanced with the buffering capacity for 32 % of granule
content. When considering chloride penetration, the effects appear to be
balanced, leading to similar values for the chloride migration at least
when using up to 32 % of granules.
The buffer capacity has no bearing on freeze-scaling. Incorporation
of granules in concrete amplifies the deterioration proportionate to the
increase in porosity. This effect is particularly noticeable during the first
exposure cycles to freeze-scaling, largely attributed to thickening of the
cement skin of concrete with the incorporation of granules. To address
the impact of the mining waste when valorised as artificial aggregate,
further study is still necessary for the life cycle assessment of this type of
granules employed in cement-based mixtures.
CRediT authorship contribution statement
Yury Villagran-Zaccardi: Writing – original draft, Visualization,
Methodology, Investigation, Formal analysis, Conceptualization. Lies­
beth Horckmans: Writing – review & editing, Resources, Project
administration, Funding acquisition, Formal analysis. Arne Peys:
Writing – review & editing, Resources, Methodology, Investigation,
Funding acquisition, Conceptualization.
Y. Villagran-Zaccardi et al.
Fig. 11. Schematic representation of the cement skin in relation with the granule content (e0, e17, and e32 are the cement skin thicknesses, and p0, p17, and p32 are
the paste contents in the bulk, correspondingly to M0, M17, and M32).
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgements
This work was carried out in the framework of the NEMO project,
funded by the European Union’s EU Framework Programme for
Research and Innovation Horizon 2020 under Grant Agreement No
776846. Collaboration of partners within the NEMO Consortium is
greatly appreciated. The support for experiments from Jo Lievens, Sten
Janssen, Bo Peeraer, Jan Van Loy, and Dirk Vanhoyweghen is greatly
appreciated.
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