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Article history: There is a growing concern on lightweight aggregates (LWA) for recycling of waste materials: this
Received 21 May 2016 manufacturing technology is considered a flexible tool to make it possible the conversion of large
Received in revised form 6 September 2016 amounts of residues into building products. The main challenge for this purpose is the control on the
Accepted 26 September 2016
technological behavior during firing of waste-bearing batches. The target is engineering the sintering
Available online 12 October 2016
and expansion of LWA in order to tailor bulk density, mechanical strength and water absorption on var-
ious possible applications (e.g., structural and non-structural lightweight concretes, lightweight mortars,
Keywords:
filtration substrates, floriculture). The prediction of the aggregate expansion – and hence the batch design
Bloating
Expansion
– is usually carried out utilizing the Riley’s and/or Cougny’s schemes, which are based on the bulk chem-
Lightweight aggregate ical composition of clay bodies. However, collecting the literature data on waste-based LWA and plotting
Waste recycling them in the Riley’s and Cougny’s diagrams, no reliable discrimination turns out between expanding and
non-expanding batches. In the same way, the attempt to modify the Riley’s and Cougny’s parameters,
including elements present in wastes but not in natural raw materials, was unsuccessful. From this stand-
point, a new approach to assess the batch expandability was developed through a deeper comprehension
of mechanisms acting on sintering and expansion of LWA. A specific characterization protocol was set up,
entailing hot-stage microscopy and determination of phase composition and microstructure. This implies
a paradigm shift from batch (chemical composition) to vitreous phase (amount, chemical composition,
and viscosity at high temperature). The vitreous phase plays a key-role for bloating, microstructure
and physical properties of LWA. A working example is presented about new LWA based on waste glasses,
ceramic tile polishing sludge and clay raw materials.
Ó 2016 Elsevier Ltd. All rights reserved.
1. Introduction tures from 1000 to 1300 °C) natural raw materials like vermiculite,
shale, clay, or slate [1]. Along with these expanded clay aggregates,
Most Lightweight Aggregates (LWA) currently on the market LWA are obtained also from naturally-occurring lightweight mate-
are manufactured by firing in rotary kilns (at maximum tempera- rials, like pumice, perlite, volcanic scoria, and cinders [1,2].
LWA have been attracting in the last decade a renovated
attention driven by the increasing demand for lightweight struc-
⇑ Corresponding author. tural materials (primarily concrete) and envelope materials with
E-mail address: michele.dondi@istec.cnr.it (M. Dondi).
http://dx.doi.org/10.1016/j.conbuildmat.2016.09.111
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409 395
improved thermal, thermo-hygrometric and acoustic perfor- prediction schemes after Riley [159] or Cougny [160]. These
mances, like lightweight mortars and external thermal insulation schemes were set up with reference to expanded clay aggregates
systems [3–6]. and expect to discriminate between ‘‘bloating” and ‘‘non-
Such a revitalized interest is further fed by the growing concern bloating” materials by defining a target field in a ternary diagram:
on sustainability, which is addressing many studies on the use of
urban and industrial wastes as possible raw materials for LWA. silica-alumina-fluxing for Riley [159], i.e. SiO2-Al2O3-
The number of papers on this matter overpassed 150 and the (Fe2O3 + MgO + CaO + Na2O + K2O);
publication rate has been increasing from 1 to 2 papers per year aluminum-iron-alkaline + alkaline earths for Cougny [160], i.e.
in the 1990s to the annual 15–20 papers of the latest years. In this Al2O3-Fe2O3-(MgO + CaO + Na2O + K2O).
literature, a wide range of waste materials were tested as partial or
total replacement of conventional raw materials for LWA. The The Riley’s field soon demonstrated less reliable than it initially
sources of such unconventional raw materials encompass munici- seemed, as amendments were proposed already in the 1960s
pal solid wastes, sediments from water reservoirs and harbor [161,162]. Despite be known that the bulk chemical composition
dredging, residues from coal power plants, mining and quarrying, is not discriminant, as materials ‘‘that expand suitably, that expand
mineral transformation and metallurgical industry (Table 1). inadequately, or that do not expand all fall in these same ranges”
These new kinds of raw materials are often characterized by [1], the ‘‘chemical design” is still a popular procedure in the LWA
chemical and mineralogical features that are far away from the batch formulation [38,52,70,84,96,123,128,131,132] and [135].
composition of clays and shales currently utilized to manufacture On the other hand, besides an increasing attention has been
expanded clay aggregates. As a consequence, waste materials paid to the factors affecting the bloating process [64,65,74,117,12
exhibit in most cases a different technological behavior – and 0,132,133,158,163,164–167] no standard protocols to evaluate
particularly a peculiar expansion behavior – with respect to the the expansion potential and firing behavior are commonly adopted
present industrial batches utilized to produce LWA [74,98]. Thus, in the design of LWA batches.
the use of wastes may impose substantial adjustments to the man- No extensive review of the novel waste-bearing LWA can be
ufacturing process in order to get the desired technical perfor- found in the literature. The purpose of the present paper is to over-
mance of LWA. These changes mainly concern the shaping and view the composition and properties of LWA produced from
firing processes, because of the different plasticity and thermal wastes and other unconventional raw materials. This first part is
behavior of unconventional raw materials [72,73,109,113,155– aimed at reappraising the expansion behavior of the numerous
157]. examples in the literature, firstly to assess whether the current
Waste-based batches represent a new combination of chemical prediction schemes are actually suitable for waste-bearing LWA
composition and processing conditions, which can bring about or not. Secondly, a new characterization protocol of the expansion
changes in the physical properties of LWA and in the ratio between behavior will be proposed and discussed.
different parameters: water absorption, total porosity, bulk den-
sity, mechanical strength. Along with the chemical composition, 2. Experimental approach
important variations may occur to both phase composition and
microstructure of LWA, with effects on amount, composition and The literature on LWA was reviewed and about 150 papers deal-
properties of the vitreous phase on one side; pore volume, pore ing with unconventional raw materials, mostly municipal and
and septum size distribution on the other side [16,21,41–43,52,5 industrial residues, came out. The spectrum of sources is extremely
8–60,86,103,146,155,158]. diversified: many studies entailed coal fly ashes, sewage-derived
The batch formulation of LWA is still designed empirically, by residues, and sediments dredged from harbors and water reser-
plotting the bulk chemical composition of raw materials into the voirs, but many different wastes were proposed as raw materials
Table 1
Waste materials proposed in the literature for LWA production.
for LWA (Table 1). Furthermore, residues were used alone or in where fluxing⁄ is (Fe2O⁄3 + MgO + CaO⁄ + Na2O + K2O + B2O3 +
mixtures of different waste sources. P2O5); Fe2O⁄3 stands for the sum of heavy metal oxides (Fe2O3,
This body of literature contains data on chemical composition, Cr2O3, MnO, PbO, ZnO); Al2O⁄3 is the sum (Al2O3 + TiO2); CaO⁄
batch processing conditions, and LWA technological properties means the sum of alkali-earth oxides (CaO + SrO + BaO).
regarding approximately 500 waste-bearing batches, which were Further elements can be present in significant amounts from
collected and elaborated. When the batch composition was not pro- both the technological (with reference to the expansion behavior)
vided, it was calculated from the chemical composition of raw mate- and the environmental points of view: carbon, sulfur, and chlorine.
rials. The set of technological features caught from the literature is Carbon was found especially in fly ash and other combustion
not uniform in terms of properties and methods followed for their residues [70,71,96,97,101]. Sulfur occurs mainly in municipal solid
determination. The properties considered include loose weight, bulk wastes [25,34]. Chlorine is present in marine sediments
density (of the single granule), real density, total porosity, water [123,143,145] and solid waste incinerator fly ashes [32,34]. How-
absorption, bloating indices, mechanical resistance (compressive ever, in the LWA manufacture, these elements undergo a partial
strength of the single granule and on pile). It was possible to contrast or almost complete volatilization during firing, depending on
the chemical composition and the bulk density for 406 batches. several factors of the process. The release of S, Cl and C into the kiln
In order to turn simpler the graphic representation of the Riley’s atmosphere occurs at different temperatures, thus it cannot be
and Cougny’s schemes, the original ternary diagrams were simply related with the bloating phenomena. For this reason, they
redrawn into binary diagrams by joining two of the three were not accounted for in the modified chemical parameters.
parameters: The database entails samples with a different degree of expan-
sion: from not expanding materials to highly bloated aggregates.
Al2O3/fluxing (Fe2O3 + MgO + CaO + Na2O + K2O) vs. SiO2 for Since the bulk density values can change upon the firing conditions
Riley [159]; (maximum temperature, soaking time, heating and pre-heating
Fe2O3/Al2O3 vs. MgO + CaO + Na2O + K2O for Cougny [160]; rates) only the best result was taken for each batch composition.
Multivariate statistical analysis of the data from literature was
the fields of ‘‘bloating clays” are reported as well (Fig. 1). carried out (software Statistica 5.1: multiple regression and facto-
However, the waste materials can contain, along with the eight rial analysis) by contrasting bulk density with chemical composi-
main components involved in the predictive schemes, also signifi- tion, as single oxides or a combination of them.
cant amounts of elements usually not considered (because in trace A protocol for the evaluation of firing behavior of LWA was set
amounts) in the case of clays and shales. These components are up in order to better predict the expansion behavior – through a
P2O5, B2O3, and heavy metals (Ba, Cr, Mn, Pb, Sr, Zn). Phosphorus simulation of the industrial processing – and to characterize funda-
is present in some units weight percent in sewage sludges mental variables, like amount and chemical composition of the
[11,13–15,37,39,43], ore beneficiation sludge [85] and some sedi- liquid phase formed at high temperature.
ments recovered by dredging harbors and water reservoirs The expansion behavior was investigated by hot-stage micro-
[45,46,126,144]. Boron is present in mining residues [84,86]. Heavy scopy (HSM, Misura 3, Expert System Solutions) which detects
metals are abundant in wastes from the metallurgical industry the morphological changes occurring to a cylindrical specimen
[31,88,96,145]. Since P2O5, B2O3, and heavy metals can remarkably (3 mm height 2 mm diameter) [168]. Two tests were performed:
influence the technological behavior of LWA batches, the original
Riley’s and Cougny’s parameters were modified to comprise these constant rate (10 °Cmin1, measuring the specimen height) to
additional components: determine the characteristic temperatures corresponding to the
end of sintering (TES); the maximum expansion (TME) whose first
Al2O⁄3 and fluxing⁄ for Riley [159]; derivative represents the temperature of maximum expansion
Fe2O⁄3, Al2O⁄3 and (MgO + CaO⁄ + Na2O + K2O + P2O5 + B2O3) for rate (TMER); ‘‘melting”, conventionally intended as the tempera-
Cougny [160]; ture to which the specimen assumes a half sphere shape (THS).
Fig. 1. Binary representations of predictive schemes for expanded clay aggregates: field of expanding (A) and highly expanding clays (B) after Riley [159]; field of expanding
clays (C) after Cougny [160].
M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409 397
Fig. 2. Bulk density of LWA from wastes in function of firing temperature (A) and water absorption (B).
Isothermal run at the temperature of maximum expansion rate cylinders and a wet grinding time of 15 min. An internal standard
(80 °Cmin1 till TMER followed by a 45 min soaking) to estimate (a-Al2O3 <1 lm, Buehler Micropolish), in amount of 20 wt%, was
the bloating index: BI = Vme/Vi, where Vme is the maximum added to each sample. Quantitative mineralogical analyses [169]
volume of the aggregate after expansion and Vi is the initial were performed using RIR/Rietveld techniques. Bruker Topas 4.2
volume of the unfired aggregate; the volume was calculated and Panalytical HighScore Plus 3.5 software packages were used.
approaching images to regular solids [52,60]. Crystal structure data and atomic coordinates of minerals for
Rietveld refinements were retrieved from the ICSD and were the
The mineralogical composition of LWA was investigated, in following: sanidine [170], albite [171], quartz [172]. Preferred ori-
order to determine residual crystalline phases, by means of X-ray entation was treated for each phases with the spherical harmonics
powder diffraction (XRPD) using a Panalytical X’Pert Pro diffrac- approach, whenever required. Amorphous content was calculated
tometer (Cu-Ka radiation, 40 kV, 40 mA, 4-50° 2h scanning inter- by difference. The chemical composition of the vitreous phase
val, 0.017° equivalent step size, 120 s per step equivalent was calculated by subtracting the contribution of crystalline
counting time, RTMS X’Celerator detector). Powders with grain size phases from the bulk composition of the fired aggregate
<10 lm were obtained using a McCrone micronizer mill with agate determined by X-ray fluorescence spectrometry (XRF-WDS, Axios,
Fig. 3. LWA from wastes in the Riley [159] predictive scheme (A) SiO2-Al2O3-(Fe2O3 + MgO + CaO + Na2O + K2O) and (B) with the modified fluxing parameter (which includes
P2O5, B2O3, and heavy metals).
398 M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409
Fig. 4. LWA from wastes in the Cougny [160] predictive scheme (A) Al2O3-Fe2O3-(MgO + CaO + Na2O + K2O) and (B) with the modified parameters (which includes P2O5, B2O3,
and heavy metals).
bulk density (0.6–1.0 gcm3) strongly decreased from 1050 to strength. On the other hand, the disappearance of pyroxene together
1100 °C. The major crystalline phases identified in the raw ash with an increasing proportion of plagioclase determine a decrease in
were quartz (SiO2), whose amount decreased on sintering, hema- the density of LWA produced with the clay-rich sediment.
tite (Fe2O3), corundum (Al2O3) and berlinite (AlPO4). The mineralogical transformations occurring in the 800–
Mixtures of natural zeolitized rocks (clinoptilolite- or chabazite- 1200 °C range were investigated for a diatomaceous clay (Moler)
rich) and SiC-bearing sludge deriving from polishing of porcelain consisting of 70% wt diatomite and 30% wt montmorillonite along
stoneware tiles were tested for the production of LWA as con- with volcanic ash layers [178]. Moler was converted mainly into
stituents of structural and/or thermo-insulating lightweight con- cristobalite in the 900–1100 °C range. Samples treated at the high-
cretes [52]. It was demonstrated that the firing expansion is est temperatures contained less mullite and hematite.
deeply depending on the occurrence of SiC in the industrial waste.
Different amounts of a powdered limestone were also added to the 3.2.3. Viscosity at high temperature of the vitreous phase
batch, resulting in an even increased expansion, though accompa- Kaz’mina et al. [89] assessed the viscosity of the glass-crystal
nied by a worsening of the mechanical properties of the LWA. Natu- composition in the LWA foaming temperature range (800–
ral zeolitized materials mixed with the industrial sludge (30% wt) 850 °C) which resulted to be higher than that of glass, because of
allowed the production of LWA with densities ranging between the occurrence of a residual crystalline phase (a form of SiO2)
0.8 and 1.0 gcm3, thus suitable for the preparation of structural which increases the viscosity. It was demonstrated that, for a
lightweight concretes. Less dense aggregates (0.6–0.7 gcm3) were glassy phase content lower than 75% wt, the viscosity of the LWA
also obtained by adding powdered limestone (10% wt) potentially body depends on the crystals-to-glassy phase ratio; for a glassy
useful for the manufacture of thermo-insulating lightweight phase content higher than 75% wt, the viscosity of the composition
concretes. and bloating index are mainly determined by the chemical compo-
The effect of MgO contents on the physical, chemical and sition of the glassy phase.
microstructural properties of LWA was assessed under controlled LWA with bottom ash from a thermal power plant and dredged
or rapid cooling [104]. Results indicate that cordierite (Mg2Al4Si5 soil were manufactured by direct sintering for 10 min at 1050–
O18) is found in LWA when the MgO content reaches 2%, along with 1200 °C [115]. The weight ratio of coal bottom ash to the dredged
a mullite decreasing. An increase in the content of basic magnesium soil is of 7:3, and 5% wt waste glass was added to the batch; fur-
carbonate in the batch generates more CO2, turning into higher thermore, Na2O was added to the waste glass up to 6% wt in order
porosity values as well as lower bulk density and compressive to control the viscosity of the vitreous phase during the heat treat-
strength of LWA pellets. The formation of cordierite was found to ment. The LWA without waste glass showed a limited bloating at
prevent the generation of cracks within LWA pellets, improving their 1200 °C, which is enhanced by the waste glass with a consequent
strength and reducing water absorption under rapid cooling decrease of the bulk density from 1.44 to 1.20 gcm3; water
conditions. absorption is in the 12–23% range.
Microstructural and mineralogical features of LWA manufac-
tured with washing sludge (WS), fly ash (FA), used motor oil and 3.2.4. Particle size
washing aggregate sludge, sewage sludge and a clay-rich sediment Particle size has to be controlled to get a compromise between a
were investigated [16,21]. The degree of vitrification of LWA is fine-grained distribution (necessary to entrap gases and promote
mostly affected by temperature and batch formulation. LWA with sintering kinetics) and a coarser distribution, needed to ensure
WS and FA generally showed an external layer and a glassy core with the proper workability of aggregates. A range of particle size distri-
isolated pores. The presence of coarser pores is related to a lower bution (Fig. 7) was proposed to obtain the best behavior in terms of
density of the unfired pellets, whilst when the external layer is lack- both expansion and technological properties of LWA [160].
ing the water absorption values were dependent on the size and Aineto and coworkers [98] analyzed vitreous slag (SL) and fly
amount of open or closed pores. The mineralogical analyses revealed ash (FA) from a gasification plant. Such wastes exhibit expanding
the formation of plagioclase and pyroxene, along with minor gehlen- properties at high temperatures due to a gas exolution from the
ite, during the heat treatment. The formation of Ca-plagioclase and glassy phase. This process, simultaneous to the devitrification of
the dissolution of quartz during firing improved the compressive crystalline phases, may result in the development of porosity that
Fig. 7. Best particle size distribution range for LWA expansion, modified after Cougny [160].
M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409 401
can be modulated by controlling the temperature of thermal treat- mediate product for foam glass crystalline materials based on silica
ments. The different behavior on the development of porosity at temperatures not exceeding 900 °C [133]. The results show that
recorded in FA and SL was explained by the finer particle size LWA produced above 1200 °C met the EN-13055-1, which states
and higher content of volatile compounds in FA, which promoted that the unit weight of LWA should be lower than 2000 kgm3.
an earlier liquid phase formation and a greater gas release and coa- The bulk density was easily lowered by extending the soaking time
lescence of bubbles with the consequent opening of the porosity. and increasing the heating rate. The ratio of strength to unit weight
LWA were prepared from rice husk ash (RHA) obtained from a of the LWA produced at 1230 °C, with a short soaking time and a
biomass power plant, containing over 80% wt. of silica and small fast heating rate, was near to that of a commercial product. The
amounts of K2O, Na2O and Fe2O3 [152]. RHA has the potential for level of water adsorption was below 4%, which increased initially
making LWA with very low bulk density (0.2–0.4 gcm3) whose and then decreased due to pore connections and pore sealing.
properties are enhanced with increasing fineness of RHA. The reac- The formation of a glassy phase in the LWA treated at higher tem-
tion of RHA with a 10 M NaOH solution (at 115 °C for 24 h to form a perature created a microstructure with rough and sealed small
sodium silicate) and following treatment to 500 °C provided better pores (<0.1 mm) connected to the walls of large pores (>0.2 mm).
LWA than the as-received RHA. The stability of LWA was obtained The effect of preheating and firing conditions on the bloating
by incorporating 2–7% wt of boric acid in the RHA mixture. mechanism was studied on LWA manufactured by dehydrated
Reservoir sediments, blended with waste glass with different sewage sludge (DSS) and clay [17]. Chemical components, espe-
degrees of fineness, were investigated to disclose how particle size cially the C/Fe ratio, were used to explain the preheating mecha-
distribution affects both the sintering behavior and LWA character- nism; physical forces (surface tension and bloating force)
istics [10]. Fine-grained glass smoothed the surface of the aggre- combined with C/Fe ratio were used to explain the bloating mech-
gates and decreased the LWA pore size, with the breaking load anism. The optimum addition of DSS was 20–30% wt, whose pellets
increasing by a 76%. Waste glass particle size >150 lm brought preheated for 20 min at 400 °C and fired for 10 min at 1150 °C were
about LWA with bulk density <1.8 gcm3; conversely, when the good to produce LWA with a bulk density of 0.3–0.8 gcm3, a
waste glass particle size was <150 lm, the LWA bulk density water absorption of 5.3% wt., and non-toxic (metal leaching data
exceeded 1.8 gcm3. The addition of the fine-grained waste glass were all below the detection limit) and suitable for practical civil
into reservoir sediment positively affects the resistance to chemi- engineering.
cal corrosion and potential alkali-silica reactivity of LWA. The effects of prefiring and firing dwell times on the chemical,
physical and microstructural properties of LWA produced from
3.2.5. Use of additives mining and industrial waste with a rotary kiln were determined
As regards additives employed to improve the bloating process, [74]. It was observed that 1.5 and 3 min of prefiring and firing
waste sludges from sawing and polishing of ornamental stones and dwell times, respectively, were more adequate than 5 and 4 min
porcelain stoneware were experimented for the manufacture of to get a lower density (0.98 vs. 1.64 gcm3).
LWA [53]. The occurrence of SiC (the abrasive component) is a
key-point, since it decomposes at high temperature with gas 3.2.7. Furnace atmosphere
release, thus acting as a bloating promoter and giving rise to Kim et al. [164] investigated LWA made of bottom ash (70% wt)
LWA with particle density <1 gcm3. Slight variations in the batch and dredged soil (30% wt) produced under various firing atmo-
composition allowed to produce LWA with different properties: spheres (oxidizing, neutral and reducing) at 1150 and 1200 °C.
e.g., high mechanical resistance (particle density 1.25 gcm3; LWA fired in oxidizing atmosphere showed a microstructure with
strength of particle 6.9 MPa). a clear border between shell and black core, while LWA fired in
The performance of three binders (ordinary Portland cement, reducing atmosphere (with a CO gas flow rate of 10 L/min) exhib-
Na-bentonite and powdered limestone) was tested on the proper- ited in cross-section only a black core area. The black core of the
ties of sintered fly ash aggregate [99]. The properties of these LWA LWA fired in neutral atmosphere was more extended when the
depend on the type of binder and its dosage; when bentonite is N2 gas flow rate increased.
added with fly ash, a significant improvement in strength and The effect of oxidizing-reducing conditions on different mixes
reduction in water absorption is observed. Although the binders based on silicate raw materials was appraised to obtain LWA
used did not substantially alter the chemical composition, they [156]. Two different coefficients were proposed: (1) the coefficient
influenced the LWA microstructure in a way that enhanced the of effective foaming Kv = (Vf Vi)/Vi, where Vf is the final volume
mechanical properties. and Vi is the initial volume; (2) the oxidation coefficient that char-
LWA were obtained from a water reservoir sediment (mainly acterizes the quantitative ratio of the oxidizers and reducers in the
composed of SiO2 61.4%, Al2O3 22.5%, and Fe2O3 8.6% wt, with vari- batch: Ko = (CORf Mf + CORo Mo)/(RCORi Mi) where COR is
ous additions of CaO) fired at temperatures of 1170–1230 °C [132]. the chemical oxygen requirement in mg for 100 g of carbon-
The addition of 1% wt. CaO to the batch calcined at 1200 °C allowed containing foaming agents for each component (f-o-i) and M is
to achieve LWA with the performance of a commercial product. CaO the mass content (% for each component f-o-i). Results showed that
addition did not promote any pozzolanic reaction and lowered Kv is strictly depending on the oxidation coefficient. Expanding
water adsorption of LWA, due to an excess of glassy phase, which mixtures fall into three groups: oxidizing (Ko < 25), transitional
sealed the pores. In contrast, the CaO addition weakened the com- (25 < Ko < 100) and reducing (Ko > 100). LWA mixes, belonging to
pressive strength. The addition of sodium carbonate to a water the transitional group, are optimal for foaming and are character-
reservoir sediment was found to form a glassy phase during the ized by a uniformly fine pore structure while for oxidizing and
heating process, while the CO2 released forms a porous structure reducing groups a high degree of structural non-uniformity is
[134]. By the addition of 5% wt Na2CO3, the firing temperature can observed.
be lowered by 100 °C, with great effect on pore formation and
growth. 3.2.8. Furnace design
Three main types of industrial furnaces are currently utilized for
3.2.6. Firing schedule, including maximum temperature, pre-heating the production of LWA: (1) rotative kiln; (2) moving grate; (3) fluid
rate and duration bed. The rotary kiln is the most important and most used in the
LWA were produced from water reservoir sediment with added industrial production; variants are possible (coaxial, with different
calcium oxide in the 1170–1230 °C range together with an inter- diameters in cascade, with variable diameter) and selected
402 M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409
according to the raw materials and LWA characteristics [160]. tives from the abrasive tools (silicon carbide and magnesium oxy-
Wainwright et al. [51] described the use of an innovative rotary chloride, MOC) on bloating at 1000–1200 °C [165]. SiC is more
kiln to produce synthetic aggregates from a variety of waste effective than MOC in the same content and firing conditions, but
streams. This Trefoil kiln has a new design supposed to be ther- the best expansion occurred with a small amount of both MOC
mally more efficient than the traditional one. Different combina- and SiC. The bloating mechanism appears to be related to SiC oxi-
tions of wastes were tested to produce LWA suitable for natural dation reaction with generation at high temperature of CO and CO2
aggregate replacement. gases:
3.3. Bloating agents: the role of evolved gases SiC þ 2O2 ! SiO2 þ CO2 " ð8Þ
Fig. 8. Expected behavior of LWA batches during hot-stage microscope runs at constant thermal rate (A) and in isothermal conditions (B). Characteristic temperatures for
start of sintering (TSS), end of sintering (TES), maximum expansion (TME), maximum expansion rate (TMER) and half sphere (THS). Bloating index as (VM V0)/V0 ratio (see text
for details).
thermal behavior, with special emphasis on the assessment of of LWA, including loose weight, water absorption, chemical and
aggregate expansion (bulk density, bloating index) in conditions mechanical resistance [53,182–184].
able to simulate those occurring in industrial furnaces by means
of a hot-stage microscope (HSM); 3.4.1. Expansion behavior
compositional features, in particular chemical composition of Expansion behavior can be investigated by HSM, which allows
the vitreous phase inferred from quantitative phase analysis to properly simulate the very fast thermal rates involved in LWA
(XRD plus Rietveld refinement) and bulk chemical composition production and to get quantitative results in terms of both charac-
of the batch (WDS-XRF or ICP-OES); teristic temperatures and expansion degree or bloating index. The
physical properties of the vitreous phase, especially viscosity at protocol requires to perform HSM runs in function of temperature
high temperature, as calculated from its chemical composition and time (Fig. 8). A first run is carried out at a constant thermal rate
by means of models set up for glasses [173]; (typically 10 °Cmin1) to get characteristic temperatures from the
microstructural features, like amount, size and shape of pores changing shape of the specimen [168]. A second run is performed
and septal thickness, as measured by image analysis on in isothermal conditions (getting as fast as possible at the temper-
micrographs taken under an optical microscope or a scanning ature of maximum expansion rate) to have information on the
electron microscope (SEM). degree of expansion over time (typically 30–45 min, i.e. a common
time taken by aggregates to roll along an industrial rotary kiln).
This protocol is thought to determine the expansion behavior of The typical firing behavior of LWA batches, in the run at constant
batches and should be integrated by technological tests (simulat- thermal rate, is inferred by the change in size (and shape) of the
ing the LWA industrial processing) and standard characterization specimen, that consists in (Fig. 8A)
Fig. 9. Examples of the behavior of different materials during hot-stage microscope runs at constant thermal rate (A) and in isothermal conditions (B).
404 M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409
Table 2
Bulk chemical and mineralogical composition of the bodies consisting of zeolite rock mining waste + ceramic tile polishing mud + scrap glass, together with the chemical
composition of the vitreous phase.
Fig. 10. (A) Estimated viscosity at the temperature of maximum expansion rate (TMER) in function of scrap glass addition. (B) Bloating index as a function of the viscosity at
the firing temperature (TFIRE) of LWA.
M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409 405
Fig. 11. Microstructure and pore distribution of LWA: as cumulative number (A), cumulative volume (B).
Fig. 12. Size distribution of septa between pores in LWA containing waste glass.
slight volume increasing, due to the natural thermal expansion a quantitative bloating index, BI = (VM V0)/V0, where V0 is the
of the material, till the start of sintering (TSS); volume of unfired specimen and VM is the maximum volume
sintering, usually by viscous flow, till the temperature of maxi- achieved;
mum densification, which corresponds to the end of sintering information on the bloating stability over the firing time: a
(TES); given batch may exhibit a stable expansion degree (keeping
bloating, due to a progressive volume growth until the temper- its BI constant for increasing time from t1 to t2) or be affected
ature of maximum expansion (TME); a temperature of maximum by unstable expansion with collapse of the aggregate (BI
expansion rate can be taken by the first derivative (TMER); decreases with time from t1 to t2).
melting point, which is conventionally taken as the temperature
of half sphere (THS). Examples of the behavior of different materials are reported in
Fig. 9. For instance, a typical commercial batch for expanded clay
The bloating behavior, as assessed in the isothermal run at the exhibits, in the constant rate run, a strong expansion (almost
TMER (Fig. 8B) allows to get: 120% of the initial specimen size) and a stable expansion, corre-
sponding to nearly 4 times the volume of the starting aggregate
a more reliable evaluation of the actual expansion (estimating a all over the isothermal run. An efficacious bloating agent, like the
volume instead of the specimen height); the volume is calcu- SiC-bearing mud from ceramic tiles polishing, is characterized by
lated approaching the specimen shape to regular polyhedra; an outstanding expansion in both runs, more accentuated than that
406 M. Dondi et al. / Construction and Building Materials 127 (2016) 394–409
of the expanded clay batch. Residues often present a limited a small glass addition (10%) did not induce significant changes in
expansion propensity, as in the case of the waste in Fig. 9, clearly the size distribution of septa (Fig. 12). Increasing amounts of glass
insufficient for LWA requirements. Nevertheless, the same waste provoked a different distribution in the VB and VS series, with LWA
material can be improved by the addition of the bloating agent, containing screen glass that have bigger septa.
turning its behavior close to that of expanded clay in the constant
rate run (Fig. 9A) and able to increase the expansion in the isother-
4. Conclusions
mal run, till a LWA volume almost 3 times the initial one (Fig. 9B).
The main challenge in the manufacture of waste-bearing LWA is
3.4.2. Compositional characterization
the control on their technological behavior during firing. Basic
A compositional characterization is fundamental to obtain a
properties (bulk density, mechanical strength and water absorp-
quantitative estimation on the amount of vitreous and crystalline
tion) that must be tailored for various applications depend on
phases present in the LWA. The bulk chemical composition of the
the actual engineering of the LWA sintering and bloating processes.
batch is needed to calculate, for every oxide, the fraction referred
Several factors play a significant role during the LWA firing, includ-
to the vitreous phase by subtracting the contribution of every crys-
ing chemical and phase composition, particle and pellet size, vis-
talline phase.
cosity of the vitreous phase, firing schedule, furnace atmosphere
A working example concerns the two residues characterized in
and design, use of additives (and particularly of bloating agents).
Fig. 9 (a zeolite rock mining waste and ceramic tile polishing mud)
It has been demonstrated, by reviewing a large body of litera-
that were admixed in the 7:3 ratio by weight. This body (V0) was
ture, that the prediction of the aggregate expansion, usually based
added with 10%, 20% or 30% wt of waste glasses (VB container
on the bulk chemical composition by the Riley’s and/or Cougny’s
scrap glass or VS screen glass from TV-PC dismantling). The bulk
schemes, is not reliable and a new approach to assess the batch
chemical composition of the seven bodies is shown in Table 2,
expandability is needed. In order to go deeper in the comprehen-
together with the chemical composition of the vitreous phase
sion of mechanisms active during expansion of LWA, a specific
obtained after subtraction of the contribution from residual phases
characterization protocol was set up, entailing hot-stage micro-
(quartz, sanidine and plagioclase).
scopy and determination of phase composition and microstructure.
The addition of soda-lime glass (VB) brought about an incre-
This implies a paradigm shift from batch (chemical composition) to
ment of CaO and Na2O (minor for SiO2) as well as a diminution
vitreous phase (amount, chemical composition, and viscosity at
of Al2O3, Fe2O3, MgO and K2O. In the case of screen glass (VS) the
high temperature). A working example with batches based on
decreasing in Al2O3, Fe2O3, MgO and CaO was compensated by an
waste glasses, ceramic tile polishing sludge and clay raw materials
increasing of Na2O, SrO and BaO (plus minor amounts of ZrO2,
confirmed the key-role of the vitreous phase for bloating,
PbO and K2O). These trends occurred in both the bulk and the vit-
microstructure and physical properties of LWA.
reous phase. When the amount of scrap glass is increased from
zero to 30% the following changes of technological behavior can
be observed: Acknowledgements
- decreasing of TMER from 1210 °C (V0) to 1170 °C (VB) and This work was supported by the Emilia-Romagna region (POR-
1110 °C (VS); FESR 2014-2020) within the project MATER_SOS (Sustainable
- increasing bulk density from 0.41 gcm3 (V0) to 0.51 gcm3 materials for restoration and construction of new buildings, CUP
(VB) and 0.62 gcm3 (VS); E32I16000020007).
- correspondent decreasing of the BI from 2.43 (V0) to 1.85 (VB)
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