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h i g h l i g h t s g r a p h i c a l a b s t r a c t
14
5h
8h
12 h
(a)
BE ABLE TO REDUCE
for the production of autoclaved
Compressive strength (MPa)
12
Silica
THE COSTS OF
10
0
100 OPERATION
aerated concrete was studied. 30
20
10
90
80
70
8
14
12 h
16 h
24 h
(b)
products.
Compressive strength (MPa)
12
10
2
Enhance the compressive strength
conditions. Porous & Lightweight Low steam pressure curing MAY COST LESS
FOR THE
Tobermorite formation and pores Long reaction time EQUIPMENT
Low temperature demand
filling are curial to the compressive
strength of autoclaved aerated
concrete.
a r t i c l e i n f o a b s t r a c t
Article history: This study describes the effects of raw mix composition, amount of foaming agent, water-solids ratio,
Received 21 March 2017 steam pressure, and curing time on the characteristics of autoclaved aerated concrete (AAC). The bulk
Received in revised form 10 July 2017 density, compressive strength, and microstructures of AAC specimens were examined, and X-ray diffrac-
Accepted 12 July 2017
tion, mercury intrusion porosimetry, and thermal analyses were employed. The bulk density of AAC was
Available online 24 July 2017
affected by the amount of aluminum powder added and water-solids ratio, and especially the latter. An
increase in the amount of cement was not beneficial to the development of compressive strength. In con-
Keywords:
trast, autoclave curing greatly enhanced the compressive strength, and the AAC specimen autoclaved at
Autoclaved aerated concrete
Composition design
12 atm for 16 h had the highest compressive strength of 13.3 MPa. Increasing steam pressure can notably
Autoclaving conditions reduce the curing time, based on similar requirements of compressive strength. In contrast, prolonging
Bulk density curing time was helpful to the development of compressive strength under low steam pressure
Compressive strength conditions.
Ó 2017 Elsevier Ltd. All rights reserved.
⇑ Corresponding author.
E-mail address: roy.yl.chen@gmail.com (Y.-L. Chen).
http://dx.doi.org/10.1016/j.conbuildmat.2017.07.116
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
Y.-L. Chen et al. / Construction and Building Materials 153 (2017) 622–629 623
type calcium silicate hydrates (CSH) will become crystalline tober- The silica-lime-cement ternary diagram of the raw mix compositions of AAC is
morite, which then enhances the material’s mechanical strength. shown in Fig. 1, based on a review of several studies on AAC production from the
The resulting material is called autoclaved aerated concrete 1980s to the present [12,16–20]. The figure shows that the differences in the
(AAC), autoclaved lightweight concrete, or autoclaved cellular amounts of lime and cement are greater than the differences in the amounts of sil-
ica. Lime and cement both varied between 5 and 30 wt%, while silica varied
concrete.
between 60 and 70 wt%. The experimental design of the AAC raw mixes in this
The basic raw materials of AAC include silica sand, lime powder, study was based on the results of literature survey, and the exact proportions of
and cement. In recent years, some substitute materials and indus- the raw materials are given in Table 1.
trial byproducts, such as coal-fired fly and bottom ashes [12,13], In order to minimize the influence of particle size, the particle size distribution
silica fume [14], mine tailing, and iron slag [15], have been studied, of raw materials was determined and controlled at the same level for all the sam-
ples. Fig. 2 shows the particle size distribution of silica, lime, and cement used for
and there exists a wide variation in the raw mix compositions sug- AAC production. The high-purity silica powder (99.5%) was purchased from Alfa
The preparation of AAC specimens can be divided into three steps: (1) raw 3.1. Bulk density and changes in characteristics
material mixing, (2) foaming and pre-curing, and (3) autoclave curing, described
as follows:
The porosity is very important to AAC, because it provides
At first, silica, lime, and cement powders were precisely weighed in accordance excellent physical properties, including thermal and sound insula-
with the experimental design (shown in Table 1) and then put into a steel tion, fire resistance, and light weight. During AAC production, the
blending bowl. Aluminum powder (Alfa Aesar, 99.5%) was employed as a foam- foaming process fundamentally decides the porous characteristic,
ing agent, and its addition amount was 0.25–1.00 wt%. The raw materials were
so the factors related to foaming should be examined. In this work,
mixed with the foaming agent by using an electric blender until the mix had
become homogeneous. the effects of the amount of aluminum powder added and water-
Secondly, water was subsequently added into a raw mix at a specific water- solids ratio on the bulk density of AAC were studied, and the
solids ratio (0.6, 0.7, 0.8, 0.9, or 1.0 L/kg) and then blended to a mortar as soon results are shown in Fig. 3. It is known that hydrogen gas is gener-
as possible. The mortar was poured into cast-iron molds (50-mm cube in shape) ated when aluminum reacts with alkaline substances, e.g. calcium
where it was allowed to expand. After standing for 30 min, the expansion of
mortar nearly finished, and then the parts bulging out of molds were scraped
hydroxide, and this makes the AAC mortars expand and conse-
off. The specimens with molds were immediately put in a moist closet where quently reduces the bulk density. The representative chemical
the relative humidity was about 95%, and the temperature was controlled at reaction of aluminum and calcium hydroxide is given in Eq. (1).
23 ± 2 °C. After pre-curing in the moist closet for 24 h, the hardened specimens
were removed from the molds. 2Al þ 3CaðOHÞ2 þ 6H2 O ! 3CaO Al2 O3 6H2 O þ 3H2 " ð1Þ
Finally, the hardened specimens were cured by using an autoclave with a pro
portional-integral-derivative controller in order to complete the hydration reac- As the amount of aluminum powder varied from 0.25 to 1.0 wt
tions, and thus AAC specimens were obtained. The autoclave curing conditions %, the AAC with different silica-lime-cement compositions (S60-
investigated in this study were temperature, steam pressure, and curing time. L25-C15, S65-L20-C15, and S70-L30-C15) showed similar results.
The temperature was controlled at 160–208 °C, while the corresponding steam The bulk density of AAC gradually decreased with the increase in
pressure varied between 6 and 18 atm. The curing time was set from 5 to 24 h.
To find out the appropriate combinations of autoclave curing conditions, the
the addition of aluminum powder, but the rate of this decrease
lower steam pressure was accompanied by a longer curing time, whereas the between 0.25 and 0.5 wt% of aluminum powder was higher than
higher steam pressure was accompanied by a shorter curing time. that above 0.5 wt%. This shows that although more foaming agent
can generate a larger amount of gas, and thus should promote the
(a) expansion of AAC mortars, not all of the gas is entrapped and the
excess escapes from the mortars. On the other hand, in comparison
with the addition of aluminum powder, the water-solids ratio had
more noticeable effects on the bulk density of AAC. The bulk den-
sity sharply decreased from about 1000 to 300 kg/m3 when the
water-solids ratio was increased from 0.6 to 1.0 L/kg. A possible
explanation for this may lie in the fact that the mortar with a
higher water-solids ratio is less viscous and therefore facilitates
the formation of air voids, further reducing the bulk density of
AAC. Once again, the silica-lime-cement composition of AAC seems
insensitive to the effect of water-solids ratio on the bulk density.
The above findings suggest that the water-solids ratio is more
important with regard to the bulk density of AAC than the amount
of aluminum powder added. In sum, a thin mortar is beneficial to
the formation of air voids, but a dense one easily entraps them,
so that an appropriate water-solids ratio is a critical factor which
needs to be identified in the initial stage of AAC production.
After foaming and pre-curing, the mortars turned into hardened
specimens, which will become AAC by further autoclave curing.
Table 2 presents the bulk density and compressive strength of
the hardened and autoclaved specimens. The bulk density of hard-
ened specimens was almost identical to that of autoclaved speci-
mens. This indicates that the bulk density of AAC is already
(b) decided in the foaming and pre-curing processes, and the autoclave
curing has little influence. However, with respect to compressive
strength, the hardened and autoclaved specimens were completely
different. The average compressive strength of the hardened spec-
imens was only 45.0–103.2 kPa, while that of autoclaved speci-
mens increased to 5.7–13.3 MPa. The results demonstrate that
autoclave curing can markedly increase the compressive strength
of AAC, even by more than one hundred times.
Fig. 4 shows the XRD patterns of the AAC raw mix, hardened
specimen, and autoclaved specimen (S60-L25-C15). In the raw
mix, quartz (SiO2) and lime (CaO) were the dominant mineral
phases, which account for 60 wt% and 25 wt%, respectively. By
mixing raw mix with water and pre-curing, the hardened specimen
was obtained and there were some changes in the mineral compo-
sition. The diffraction peaks of lime almost disappeared and port-
landite, Ca(OH)2, substituted for lime. After autoclave curing, the
portlandite vanished and a crystalline hydrate, tobermorite (Ca5(-
OH)2Si6O164H2O), formed in the specimen. In addition, the inten-
sity of the diffraction peaks of quartz slightly decreased, which
implies that the quantity of quartz partially diminished. Under a
high-pressure steam condition, some studies [24,25] suggested
Fig. 3. Bulk density of the AAC specimens produced with different amounts of
that tobermorite was produced from amorphous CSH whereas
aluminum powder added and water-solids ratios. another [26] reported that tobermorite can be formed by the reac-
tion of Ca(OH)2 and SiO2. The results of this study appear to be con-
sistent with the latter, and in this work there was very little
Table 2
Bulk density and compressive strength of the hardened and autoclaved specimens.
Fig. 5. Compressive strength of the AAC specimens autoclaved at 12 atm for 5–24 h.
Fig. 7. Correlation between apparent porosity and bulk density of AAC specimens.
Fig. 6. Compressive strength of the AAC specimens (S70-L25-C05) autoclaved at Fig. 8. XRD patterns of the S70-L25-C05 specimens autoclaved at 12 atm for 5, 12,
different steam pressures and curing times. and16 h.
628 Y.-L. Chen et al. / Construction and Building Materials 153 (2017) 622–629
Fig. 9 presents the TG and DSC curves of the S70-L25-C05 spec- DSC curve of an AAC specimen, i.e. two endothermic peaks accom-
imens autoclaved at 12 atm for 5, 12, and 16 h. Alarcon-Ruiz et al. panied by the loss of weight and one exothermic peak. The
[28] used the thermal analysis to examine cement pastes and endothermic peak at 400–500 °C is related to the decomposition
described the reactions that occur with increasing temperatures of Ca(OH)2, and the other endothermic peak located around
in cement pastes and concrete materials. In the temperature range 700 °C is attributed to the decarbonation of CaCO3. Both Ca(OH)2
of 180–300 °C, CSH was decomposed and lost the bound water. In and CaCO3 can be regarded as unreacted calcium compounds per-
this study, the weight loss related to CSH is between 1.67 and sisting in the AAC specimens. As the autoclave curing time
2.23 wt%, a finding which shows that only a small amount of CSH increased from 5 to 16 h, the peaks related to Ca(OH)2 and CaCO3
was present after autoclave curing. In addition to the decomposi- became smaller and smaller, a finding which means that the
tion of CSH, it is found that there are three obvious peaks in a hydration reactions in the AAC specimens tend to be complete.
The decrease in Ca(OH)2 is in accordance with the observation in
the XRD analysis (Fig. 8). On the other hand, a large exothermic
peak was observed in a DSC curve at about 850 °C, and there was
no significant variation in weight present near the temperature.
Connan et al. [29] used thermal analysis to characterize an auto-
claved cement and indicated that an exothermic reaction occurring
at about 800–900 °C was related to the crystallization of beta-
wollastonite (b-CaSiO3) from CSH and tobermorite. Since the CSH
was insignificant in the AAC specimens, the exothermic reaction
was mainly attributed to tobermorite. Moreover, Connan et al.
[29] indicated that the integrated area and height of the exother-
mic peak correlated closely with the level of compressive strength.
In Fig. 9, the exothermic peak related to beta-wollastonite became
more significant when the curing time was increased. The results
suggest that the amount of tobermorite in the AAC specimens
increases when prolonging the curing time from 5 to 16 h, and this
should be an explanation for the enhancement of compressive
strength mentioned above.
The pore size distribution of the hardened and autoclaved spec-
imens was examined by means of the MIP analysis to understand
the variations in microstructure ascribed to the autoclave curing,
and the analysis results are given in Fig. 10. It is noted that the pore
size in the hardened specimen was mainly distributed in the range
from 101 to 100 lm, while that in the autoclaved specimens was
mostly below 101 lm. Some studies also reported a similar pore
size distribution of materials after autoclaving [30,31]. The results
show that the pores which are initially formed are further filled
with the hydration products generated during the autoclave cur-
ing. In addition, the amount of fine pores between 102 and
2 102 lm was enhanced when the curing time increased from
12 to 16 h, and this may account in part for the improvement in
the compressive strength of AAC due to the prolongation of curing
Fig. 9. TG and DSC curves of the S70-L25-C05 specimens autoclaved at 12 atm for 5, time. Nambiar and Ramamurthy [11] indicated that a negative cor-
12,and 16 h. relation exists between the compressive strength and pore size of
Fig. 10. Pore size distribution of the hardened and autoclaved specimens (S70-L25-C05).
Y.-L. Chen et al. / Construction and Building Materials 153 (2017) 622–629 629
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