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Article history: In this research both the microstructure and thickness of the interfacial transition zone (ITZ) in concretes
Received 9 September 2016 of Portland cement and lightweight aggregates (LWA) are studied. It has been established that the
Received in revised form 23 December 2016 microstructure in the ITZ strongly depends on the nature of the aggregate, specifically its porosity and
Accepted 25 January 2017
water absorption. This study aims at researching the influence of physical properties such as density,
porosity and morphology of lightweight aggregates such as pumice and expanded clays, on the
microstructure and thickness of ITZ, and determine the effect that these factors have in turn on the
Keywords:
mechanical properties as compressive strength of lightweight concretes (LWC). Lightweight aggregates
Lightweight aggregates
Lightweight concrete
were characterized by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and X-ray
ITZ microstructure Fluorescence (XRF), to determine their mineralogical, morphological and chemical characteristics. The
Lightweight concrete compressive strength characterization of ITZ by SEM-EDS, and conventional optical microscopy, was carried out on specimens
of concrete manufactured with LWA and with a conventional aggregate, in order to evaluate its thickness;
furthermore, to determine the porosity, digital image processing (DIP) was performed. Lightweight aggre-
gates contributed to the formation of a dense and thinner ITZ, when compare to the ITZ of a conventional
concrete. The lower porosity and greater amount of hydrated cement phases in the ITZ of lightweight
aggregates are attributed to their physical, morphological properties and chemical and mineralogical
composition; which contributed to the decrease of the wall effect, gestating from its surface the
formation of C-S-H, achieving interlacing of hydrated phases on the surface of these aggregates with
the cementitious matrix.
Ó 2017 Elsevier Ltd. All rights reserved.
1. Introduction particles of the aggregate, ‘‘the wall effect”; consequently, the ITZ
has a much higher porosity (2 to 3 times) than that of the hardened
The ITZ is a layer formed between an aggregate and the matrix cement paste farthest from the aggregate particles [2]. The ITZ
of cement paste, composed of a double layer ‘‘duplex film” of cal- properties are affected by the characteristics of the aggregate and
cium hydroxide crystals (Ca(OH)2) oriented to the aggregate’s side the cementitious matrix, as well. Several researchers have found
and hydrated calcium silicate, C-S-H gel, oriented to the side of the that the grain size distribution of the cement, the water cement
paste, with a thickness of about 1 lm. Farthest from the aggregates ratio, the aggregate size, and the type of aggregate have important
is the main interface zone of about 40–50 lm thick, containing effects on the ITZ properties [1–4].
larger crystals of calcium hydroxide [1]. In this zone the cement Significant efforts have been devoted to optimizing the dosage
particles are unable to bind intimately with the relatively large and to the study of mechanical properties of lightweight concrete
(LWC), to make them competent with normal weight concretes
⇑ Corresponding author. [5–7], which have led to the study of ITZ microstructure [3,4,8–11].
E-mail address: jitobon@unal.edu.co (J.I. Tobón). Finding that the mechanisms responsible for the ITZ formation
http://dx.doi.org/10.1016/j.conbuildmat.2017.01.101
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
382 P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389
are related among others with absorption and water release, which process stopped, drying the samples in an oven at 60 °C and
is a feature of the lightweight aggregates (LWA) themselves, due to afterwards they were taken for cutting, the sub samples of 2 cm2
their usual high porosity. They have higher absorption and subse- for ITZ morphological analysis. The SEM micrographs were per-
quent release of water, increasing the hydration degree of the paste formed in a SEM JEOL JSM 5910LV with detectors of backscattering
around the aggregate and the amount of free water, making the electrons and applying 15 kV to image generation and a working
adjacent paste to develop a structure with greater porosity [7,8]. distance of 10 mm. The samples were subjected to high vacuum
It is often assumed that the LWA used in the manufacture of con- and were then coated with an 8 nm layer of gold-palladium to
crete have less chemical reactivity and their interaction with the enhance their electrical conductivity. Micrographs were taken in
cement matrix is mainly physical [7]; therefore, the chemical influ- a Nikon stereoscope reference Eclipse LV100, objectives 2x, up to
ence of the LWA on the ITZ properties have received less attention. 11.5x, the stereoscopy micrographs allowed digital image
Researches carried out by Elsharief et al. and Xiao et al. [3,4] processing (DIP) for the porosimetry analysis; which describes
state that both size and texture of the aggregates surface have the pores in a section of the aggregate, when adding all images it
great influence on the ITZ properties. Authors like Yu et al. [12], is sought to recreate the pores area of a complete aggregate.
along with Kong et al. [13]; denote that both physical and chemical
interactions that occur between LWA and the cement paste are 2.2. Materials and characterization
responsible for the ITZ mechanical strength.
Some studies have shown that the water absorption and degree In the development of this study a normal weight conventional
of LWA pre-wetting may influence the interface formation process aggregate (CO) and two LWA, pumice (PO), thermally expanded
[9]; however, further research is needed to fully understand the clay, aliven (AL) and Portland cement type I (OPC) were used. In
chemical and physical process between the LWA and cement paste, Table 1 is shown the chemical composition of each one obtained
which depends on the mineralogical composition, the texture and by XRF.
shape of the aggregates, as well. It appears that the rougher the The chemical composition of aggregates corresponds to silicon
aggregate the larger the contact surface with the cement paste, oxide, aluminium oxide, iron oxide, and in lesser proportion mag-
and thus, greater adhesion [14,5,15,16]. nesium, sodium, calcium, and potassium oxides.
This paper focuses on the study of the incidence of the morphol- The mineralogical composition for the aggregates is given in the
ogy and composition (chemical and mineralogical) of the LWA in diffractograms of Figs. 1–3. In Fig. 1, can be seen that for the
the formation of ITZ microstructure and thickness, and also its pumice a broad peak is formed just between positions 2h in 20°
influence on the LWC compressive strength, seeking to develop and 30°, where the characteristic peak of quartz is around 26.5°,
structural lightweight concretes.
Table 1
Chemical composition of aggregates and cement.
2. Materials and methods
Chemical composition Weight%
2.1. Methodology PO AL CO OPC
Silicon Oxide (SiO2) 72.1 59.67 58.43 20.9
The chemical characterization of raw materials was performed Aluminum oxide (Al2 O3) 13.35 16.95 13.46 4.72
through X-ray Fluorescence (XRF), using a Panalytical equipment; Iron oxide (Fe2 O3) 1.30 9.79 8.33 3.20
model Axios, through quantitative analysis over pearl per X-ray Magnesium oxide (MgO) 0.05 4.13 6.00 1.80
Calcium oxide (CaO) 1.22 3.57 7.17 60.69
Fluorescence per dispersive wavelength.
Sodium oxide (Na2O) 3.35 2.07 1.89 0.37
The mineralogical analysis was performed in an equipment of Potassium oxide (K2O) 4.63 1.28 1.02 0.61
X-ray Diffraction (XRD) reference Panalytical X Pert PRO MPD, in Sulfur oxide (SO3) 0.08 0.04 0.09 0.13
an interval 2h between 4° and 70°, with a passage of 0.02° and Ignition losses at 2.93 0.75 2.40 3.68
an accumulation time of 56 s. A copper anode with Ka = 1.5406 Å 1000 °C
was used.
The physical properties of aggregates, such as surface area were
performed through BET test by chemisorption, the water absorp-
tion in compliance with ACI 211.2, [18] and the density is appropri-
ate to ASTM C127, [19]. The shape index (Ia) was calculated by the
procedure established in the ASTM D3398 standard [20].
The concrete mixture design was performed in compliance with
ACI 213R-03 [23]. Aggregate concrete specimens and Portland
cement type I were prepared. The dosage of cement was 500 kg/m3,
the aggregate was 400 kg/m3. The water cement ratio was varied
in 0.35 and 0.45. To achieve as the response variable the concrete
density and afterwards the compressive strength at 28 days.
The encoding used for the name of the mixtures corresponds to
the abbreviation of the aggregate used: pumice (PO), aliven (AL)
and conventional (CO), followed by the water/cement ratio of the
mixture, 0.35 or 0.45. Once the concrete specimens were fabricated
they were taken to 28 days curing as suggested by ASTM C511 [24],
in immersion in water saturated with lime (Ca(OH)2). After
reaching the age of curing, the compressive strength test to the
corresponding samples was conducted in compliance with ASTM
C109 standard [25], at ages 3 and 28 days of curing.
Taking micrographs was performed using both optical micro-
scopy and Scanning Electron Microscopy (SEM), the hydration Fig. 1. LWA pumice diffractogram.
P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389 383
Table 2
Physical properties of aggregates.
Aggregate Surface area (m2/g) Shape index (%) Density (kg/m3) Water absorption (%) Pores area DIP (%)
PO 2.10 21.2 304.8 44.0 63.2
AL 1.13 23.9 519.9 10.3 70.5
CO 0.78 24.8 1636.0 1.5 2.8
*
Particle size 7.5 mm.
Fig. 4. Pumice lightweight aggregate. (A and B) Stereoscope micrograph on the surface. (C) SEM micrograph inside the aggregate.
384 P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389
Edge
Inside aggregate
Fig. 5. Aliven lightweight aggregate. (A) Stetoscope micrograph on surface (B) Stetoscope micrograph inside, (C) SEM micrograph on the edge and inside the aggregate.
of higher size in which the water that managed to permeate the color than that of the cementitious matrix and of irregular thick-
vitrified layer is retained. Concerning the conventional aggregate, ness. The images called B are always showing a detail of ITZ that
it preserves the relationship between the porosity area and since is highlighted in red in image A.
the absorption is much lower it preserves its porosity inside; its Fig. 7 shows that in the pumice aggregates, the ITZ is difficult to
absorption is also much lower compared to LWA. define due to their light colors and their surface porosity, which
The specific area (Table 2) increases with the porosity of the allows the cement grains staying in the pores and initiate their
aggregate surface, since the pumice is an aggregate of exposed hydration from this zone with deposition of CH [15].
porosity on its surface it has more surface area compared to both Regarding the Aliven (Fig. 8) the ITZ can be seen well defined,
Aliven and conventional. In turn the porosity is associated with due to the color of the aggregate and its spherical morphology.
the density of the aggregates, the higher the porosity the lower Concerning the conventional aggregates, the ITZ is also clearly
the density of the LWA. distinguishable (Fig. 9).
The shape index for pumice corresponds to an aggregate of The micrographs obtained using SEM (Fig. 10), show C-S-H for-
morphology in poorly defined angular blocks, with little flat faces mation in the ITZ and inside the pores of the LWA of pumice, the
and hardly distinguishable blunt edges. The Aliven is mostly spher- formation of this phase is favored by the increasing amount of
ical with some oval particles. Varying Aliven morphology is due to water in the ITZ and the possibility that cement particles are
the expansion process in the rotatory oven. The conventional deposited in the pores of the LWA surface. Additionally, a poz-
aggregate comes from a mixture of particles of oval and angular zolanic reaction could be occurring between the aggregate and
shapes, present in the reservoir and angular particles product of the cement hydration products, due to high silica contents and
grinding. It has a shape index value of (24.8%) similar to Aliven, low pumice crystallinity. This can be confirmed in the
indicating spherically shaped particles [21]. Figs. 11C, 12B and C which show the formation of the greater
To minimize the effect of aggregate size on the ITZ thickness [3], amount of crystals of CH in the ITZ of aliven concrete and conven-
it was decided to use only the sizes that went through the sieve of tional concrete.
3/800 (9.5 mm) and retained in the sieve N° 4 (4.76 mm), limit of Regarding the Aliven (Fig. 11), the formation of C-S-H and CH in
aggregate from coarse to fine, as established by ASTM C330 [22]. the ITZ is observed, the hydration products of cement can pene-
trate the cavities or pores of the aggregate surface, acting as several
3. Results and discussion ‘‘hooks” binding both matrix and aggregate, known as mechanical
interlacing [8,27]. In the Aliven, the expansion temperature may
3.1. ITZ morphology cause recrystallization of its components, reducing the possibility
of pozzolanic reactivity of the surface of these aggregates.
In Figs. 7–9 are shown the ITZ around the different aggregates in In Fig. 12, it can be seen that for the concretes of conventional
the concretes evaluated. This corresponds to an aura of lighter aggregates there is more porosity in the ITZ, also a continuous
P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389 385
Fig. 7. (A) ITZ formation at 28 days of curing pumice concrete (B) Enlargement of Framed area.
Fig. 8. (A) ITZ formation at 28 days of curing Aliven concrete. (B) Enlargement of Framed area.
Fig. 9. (A) ITZ formation at 28 days of curing conventional concrete. (B) Enlargement of Framed area.
ITZ
ITZ
Matrix
Aggregate
C-S-H
A B
Fig. 10. (A) ITZ SEM micrograph sample POC5-0.35. (B) Framed area extension sample POC5-0.35.
386 P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389
ITZ
ITZ ITZ
Matrix
C-S-H CH
Aggregate
A B C
Fig. 11. (A) ITZ SEM micrograph sample ALC5-0.45 (B) Framed area extension sample ALC5-0.45 (C) sample ALC5-0.45ITZ.
Aggregate
ITZ
Eringite CH
CH
ITZ
A Matrix B C
Fig. 12. (A) ITZ SEM micrograph sample COC5-0.35 (B) sample COC5-0.35 (C) sample COC5-0.35.
direction (Fig. 12). These hydration products are mainly CH, since
the Ca+2 ions have a relatively high mobility in the solution and
tend to diffuse in the more porous zone of ITZ (due to higher con-
centration gradients in this zone), resulting in the precipitation of
CH and hydration products of calcium trisulfoaluminate as ettrin-
gite, which has been raised by authors like Garboczi & Bentz [27].
cracked cementitious
matrix
Fig. 16. Representation failure in LWC, after testing compressive strength at 28 days of curing.
388 P. Vargas et al. / Construction and Building Materials 137 (2017) 381–389
conventional
aggregate
Fig. 17. Failure in conventional concrete, after testing compressive strength at 28 days of curing.
as fine aggregate. Densities lower than 1920 kg/m3 (ACI 213-03) and innovation in postgraduate studies at Universidad Nacional de
were also achieved [23]. Colombia 2013-2015”, Code 25867.
4. Conclusions References
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