Tran Minh Duc - Anh Huong Cua Cho Do Duong Ho Nhiet Den Tinh Chat Cua Bun Do

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Construction and Building Materials 259 (2020) 119779

Contents lists available at ScienceDirect

Construction and Building Materials


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

Effect of curing regime on properties of red mud based alkali activated


materials
Minh Duc Hoang a,⇑, Quang Minh Do b, Van Quang Le c
a
Vietnam Institute for Building Science and Technology, 81 Tran Cung - Cau Giay, Hanoi, Viet Nam
b
Ho Chi Minh City University of Technology, 268 Ly Thuong Kiet - Q10, Ho Chi Minh City, Viet Nam
c
Vietnam Institute for Building Materials, 235 Nguyen Trai - Thanh Xuan, Hanoi, Viet Nam

h i g h l i g h t s

 Properties of red mud in Vietnam’s Tan Rai Alumina plant.


 Dissolution ratio of SiO2 and Al2O3 in red mud, fly ash under different conditions.
 Properties of red mud based alkali activated material after high temperature and autoclave curing.
 Regression between the compressive strength and the total amount of dissolved SiO2.

a r t i c l e i n f o a b s t r a c t

Article history: To produce the alkali activated material, red mud must be used with components containing active sil-
Received 29 July 2019 icon dioxide because silicon dioxide in red mud does not dissolve in alkaline solution. The test results
Received in revised form 12 May 2020 presented in this paper show that high pressure and high temperature treatment in an autoclave can dis-
Accepted 30 May 2020
solve part of the silicone dioxide in red mud and improve the properties of material. The compressive
strength of red mud based alkali activated materials can reach 10.6 MPa with a softening coefficient over
0.70. Adding an active silicon dioxide supplement by replacing 26.3 wt% red mud with fly ash increases
Keywords:
the compressive strength up to 20 MPa and the softening coefficient by more than 0.90. Furthermore,
Alkali activated material
Autoclave
autoclave treatment reduces residual sodium hydroxide and lowers the pH value of material. As the
Red mud result, red mud based and red mud-fly ash based alkali activated materials can be used for manufacturing
Fly ash of masonry units.
Compressive strength Ó 2020 Elsevier Ltd. All rights reserved.
Softening coefficient

1. Introduction improvement can be achieved by using up to 40 wt% of red mud in


the total amount of geopolymer. However, the strength of the
The production of alumina from bauxite by using Bayer process geopolymer was only improved with the volume of red mud in
in Vietnam poses a major environmental challenge in red mud the range of 5 wt% to 20 wt%. The reaction rate depended on the
waste’s treatment. Red mud was recycled in many ways, among NaOH concentration, but the mechanical properties depended
that using red mud to produce building materials has attracted not only on NaOH concentration, but also on other factors such
great attention from researchers. Red mud is used in the produc- as dissolution ability of the silicate and the presence of iron oxide.
tion of ceramic [1,2], clay bricks [3], in the manufacture of cement, In [13] Zhang M. used up to 20 wt% red mud with activated fly ash
concrete [4] and, in geopolymer or alkaline activated materials [1– in NaOH solution and cured at 80 °C. The result showed a signifi-
5]. In geopolymer or alkaline activated material, red mud is used in cant effect of aluminate content and amorphous silicate as well
conjunction with components containing active silicone dioxide as particle size of fly ash to the properties of the geopolymer. Zhang
such as metakaolin [5–7], rice hush ash [8,9], ground granulated M. et al. [14,15] also investigated the effect of curing conditions on
blast-furnace slag [10,11], fly ash [12–15]. the formation of geopolymer gel and properties of red mud-fly ash
In [12] Kumar A. et al. investigated the effect of red mud in fly geopolymer. They also showed the important role of curing tem-
ash based geopolymers. The result showed that geopolymerization perature in the reaction kinetic and the development of the prop-
erties of the materials.
⇑ Corresponding author. He J. [8] used red mud with fly ash, rice husk ash to produced
E-mail address: hmduc@yahoo.com (M.D. Hoang). geopolymers. He used 20 wt% to 80 wt% of red mud in combination

https://doi.org/10.1016/j.conbuildmat.2020.119779
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 M.D. Hoang et al. / Construction and Building Materials 259 (2020) 119779

with activated fly ash in the solution of water glass 1.5 M and activated by NaOH. The results showed that the curing pressure
NaOH to achieve geopolymer with compressive strengths of has a major influence on the structure formation and properties
13 MPa to 7 MPa, respectively. Geopolymer with a compressive of the geopolymer. The treatment of geopolymers including sample
strength of 20.5 MPa can be produced by adding 30 wt% to drying, high pressure curing and post-drying, leading to increased
60 wt% rice husk ash to red mud and 2 M to 6 M NaOH solution. geopolymer strength by 25%.
Smita S. et al. [11] used 30 wt% to 90 wt% red mud with fly ash Research on the influence of autoclave curing on red mud based
and GBFS activated in 6 M to 10 M NaOH solution and achieved alkaline activated materials have been limited. However, it could
geopolymers with compressive strengths ranging from 9.4 MPa be assumed that the high pressure and high temperature curing
to 35.8 MPa, respectively. in an autoclave could activate SiO2 in red mud in the presence of
In the above studies, red mud was used in combination with a residual NaOH solution. Thus, it is possible to utilize all needed
material containing active silicate and aluminate, thus red mud materials in red mud to produce alkaline activated materials with-
did not play the decisive role in geopolymerization reaction. The out using additional components. To improve the properties of the
results also showed that the higher red mud content in geopoly- materials, additional alkalis and amorphous SiO2 containing mate-
mer, the lower were the strengths of geopolymers. The SiO2 in rials such as fly ash, silica fume can be used.
the red mud did not participate in geopolymerization because it The aim of this study was to use red mud in producing alkaline
was insoluble in NaOH. Al2O3 and Fe2O3 were soluble in NaOH activated materials for masonry units with target compressive
but they had different effects on geopolymerization. While Al2O3 strength over 7.5 MPa and a softening coefficient above 0.85.
contributed to the polymer chains and played a positive role, Choi
S.C. and Lee W.K. [16] suggested that Fe2O3 inhibited the geopoly-
2. Materials and methods
merization of mine tailing, melting slag, and alkali activator. Add-
ing 5 wt% Fe2O3 by volume could lead to compressive strength
The red mud used in this study was from the Tan Rai alumina
reduction of the geopolymer from 73.6 MPa to 32.5 MPa.
plant (Vietnam). The Tan Rai alumina plant also operates a coal-
Sankar K. et al. studied the sodium silicate activated slag-fly ash
burning power plant with a capacity of 30 MW, from which the
binders and showed the formation of calcium silicate hydrate (C–
class F fly ash was used as a SiO2 supplement material. The compo-
S–H), calcium aluminum silicate hydrate (C–A–S–H) and (Ca, Na)
sition and properties of these materials are shown in Table 1.
based geopolymer [17]. The proportion of geopolymer was gener-
The total Na2O content was determined and is presented in
ally higher in slag-metakaolin binders when compared to slag-fly
Table 1. However, the Na2O content in water extract of red mud
ash binders, and the C–N–A–S–H was the major product phase
and fly ash were 0.664% and 0.010%, respectively. X-ray diffraction
[18]. They suggested the formation of soft gel in the first stage,
analysis (Fig. 1) showed that red mud contained 21% goethite
then it eventually gained strength and got hardened. The soft gel
(FeOOH), 14% hematite (Fe2O3), 5% gibbsite (Al(OH)3) and 60%
contained a modified calcium silicate hydrate gel (C–N–S–H where
amorphous phase. Fly ash contained 20% mullite (Al6Si2O13), 2%
N=Na) with a short mean chain length and no observable Al incor-
quartz (SiO2) and 78% amorphous phase.
poration [19].
The activator was prepared by dissolving 97%-98% pure NaOH
Increase of the alkaline concentration of activator could help to
pellets from the Bien Hoa Chemical Company in deionized water.
enhance the reaction and thus lead to the gain of compressive
Determination of the SiO2 and Al2O3 dissolution ratios was carried
strength of the material. However, higher alkaline concentration
out on oven dried materials that passing 0.09 mm sieve. 2.5 g of the
of activator caused higher soluble alkaline residual content in the
sample of red mud or fly ash was added to the reactor with 25 ml
material and higher risk of efflorescence (formation of sodium car-
of NaOH solution in different concentrations. A certain amount of
bonate heptahydrate Na2CO37H2O on or near the surface of the
Na2O was added to a sample of fly ash to equal its content to
material). Proper selection, proportioning of materials and high
Na2O content in red mud. The products of the reaction under dif-
temperature curing can reduce the efflorescence but could not
ferent conditions were analyzed to determine the dissolution
totally resolve the problem [20].
oxides.
The composition of the red mud depended on the plant and
A red mud based alkaline activated mixture was made by mix-
comprised of Fe2O3 (30%–60%), Al2O3, (10%–20%), SiO2 (3%–50%),
ing ingredients in a predefined proportion. A 90x80x40 mm spec-
Na2O (2%–10%), CaO (2%–8%) and other oxides with about 20%-
imen was made by semi-dry pressing under 10 N/mm2. The
30% amorphous phase. However, SiO2 in red mud could not be acti-
samples were demolded and put into high temperature curing or
vated by alkaline solution in atmospheric pressure conditions and
autoclave curing conforming to the prescribed regimes. The heat-
the formation of alkaline activated material or geopolymer cannot
ing and cooling rates of the autoclave profile were kept constantly.
occur.
The corresponding maximum pressure and temperature as well as
It was shown in [21] that under high pressure and high temper-
atures in an autoclave, crystalline SiO2 may also involve in the for-
mation of new substances. This technology was used by some Table 1
researchers for geopolymer materials [22–24]. Characteristics of raw materials.
The study by Kriven W.M. [22] on geopolymers using metakao- No. Characteristics Materials
lin and silica fume activated by NaOH and KOH solutions with rein-
Red mud Fly ash
forced fiber under high pressure and high temperature curing
1 Density, g/cm3 3.47 2.20
conditions showed that geopolymers structure became denser
2 Bulk density, kg/m3 685 905
when treated under atmospheric pressure conditions. 3 Mean particle size, lm 9.5 48.2
Kani E.N. et al. [23] produced geopolymers from natural puz- 4 Oxide content, %
zolan with a compressive strength of 108.7 MPa after high pressure - SiO2 7.40 47.74
treatment within 30 h at 210 °C following curing for 7 days at room - Al2O3 13.65 35.36
- Fe2O3 56.05 7.02
temperature and atmospheric pressure. Meanwhile, the highest - Na2O 3.63 0.69
compressive strength achieved for hydrothermal treatment at - K2O 0.25 0.41
85 °C is only 57.5 MPa. - CaO 3.10 4.20
Hanayneh B. [24] studied the effect of the curing pressure on - TiO2 0.15 0.43
- L.O.I 12.50 3.85
the properties of geopolymers using metakaolin and quartz sand
M.D. Hoang et al. / Construction and Building Materials 259 (2020) 119779 3

When heating without adding NaOH, a certain amount of SiO2


was also dissolved since the materials already contained Na2O.
SiO2 in the red mud began to dissolve when we increased the
pressure (Table 3). The dissolution ratio of SiO2 in red mud after
10 h of isothermal curing in an autoclave raised from 0.34% to
2.25% corresponding to the pressure increase from 0.4 MPa (max-
imum temperature of 144 °C) to 1.6 MPa (maximum temperature
of 201 °C). At a constant pressure of 1.2 MPa (maximum tempera-
ture of 188 °C), SiO2 dissolution ratio increased from 1.46% to 2.71%
as a result of increasing dwell time from 4 h to 16 h. Addition of
NaOH also increased the SiO2 dissolved in red mud after autoclave
curing. This result also showed that, with the same concentration
of NaOH solution, the dissolution ratio of SiO2 in red mud after
autoclave curing reached and exceeded the dissolution ratio of
SiO2 in fly ash after high temperature curing. This finding allows
us to predict that red mud under autoclave curing can be involved
Fig. 1. XRD spectra of red mud and fly ash. C – cristobalite, M – mullite, Q – quartz, in synthesis reaction similar to fly ash under high temperature
Go – goethite, H – hematite, Gi – Gibbsite. (For interpretation of the references to curing.
colour in this figure legend, the reader is referred to the web version of this article.)
High pressure and high temperature curing in an autoclave also
affected the increment of dissolution ratio. The dissolution ratio of
the dwell time were changed accordingly to an experimental plan. SiO2 was significantly increased when we raised either pressure
After autoclave treatment, the samples were maintained in a room (and temperature) or dwell time. Increasing the pressure to
condition for 28 days. 1.6 MPa (temperature to 201 °C) could double the ratio (from
4.37% to 8.45%) after 10 h curing with 1 M NaOH. While reducing
the concentration of NaOH solution, the same SiO2 dissolution ratio
3. Influence of curing regime on dissolution ability of SiO2 and can be achieved by heating at higher temperature and pressure to
Al2O3 activate the material. This method not only saved raw material
costs but also improved working conditions and protected environ-
The dissolution process of SiO2 and Al2O3 plays an important ment by reducing the consumed NaOH. Furthermore, fly ash can be
role in the synthesis process and critically affected the properties used to replace part of the red mud to provide a more active SiO2
of the materials. This study investigated the solubility of the above source for synthesis reaction and hence improve the properties
oxides in red mud and fly ash under different conditions. Tables 2 of the material.
and 3 show dissolution ratios of oxides after high temperature cur- Unlike SiO2, aluminum oxide Al2O3 in red mud and fly ash can
ing (under atmospheric pressure) and autoclave curing, be dissolved in any condition. In atmospheric pressure conditions,
respectively. the solubility of Al2O3 was less dependent on the concentration of
The results show that in the high temperature curing regime, NaOH. Raising the concentration of NaOH solution from 1 M to
SiO2 in red mud did not dissolve when the concentration of NaOH 15 M, after 24 h at 80 °C, the Al2O3 dissolution ratio in red mud
solution increased from 1 M to 15 M. The dissolution process was and fly ash increased from 4.13% to 4.76% for red mud and from
also not activated when the reaction temperature increased from 4.56% to 4.76% for fly ash. However, the increment was not linear.
80 °C to 200 °C. Meanwhile, the dissolution ratio of SiO2 in fly The Al2O3 ratio did not change when concentration of NaOH solu-
ash after 24 h curing at 80 °C sharply increased from 2.33% to tion increased from 5 M to 15 M for red mud and from 7 M to 15 M
15.21% when raising the concentration of NaOH solution from for fly ash. Increasing curing temperature significantly raised the
1 M to 15 M. Raising the temperature from 80 °C to 200 °C solubility of Al2O3. This was proven by the fact that when the cur-
increased the soluble SiO2 content in fly ash by a smaller rate. With ing temperature increased from 50 °C to 200 °C, after 10 h curing,
a reaction time of 10 h, this ratio increased from 3.23% to 4.37%. the soluble Al2O3 content in the red mud raised from 1.20% to

Table 2
Dissolution ability of SiO2 and Al2O3 after high temperature curing.

Curing regimes NaOH conc. add. Dissolution ratio, % of


T, °C s, h Red mud Fly ash
SiO2 Al2O3 SiO2 Al2O3
80 24 1M 0.00 4.13 2.33 4.56
80 24 3M 0.00 4.74 4.58 4.66
80 24 5M 0.00 4.76 8.66 4.70
80 24 7M 0.00 4.76 10.65 4.76
80 24 9M 0.00 4.76 13.68 4.76
80 24 11M 0.00 4.76 14.98 4.76
80 24 13M 0.00 4.76 15.15 4.76
80 24 15M 0.00 4.76 15.21 4.76
50 10 – 0.00 1.20 1.06 1.47
100 10 – 0.00 2.20 1.41 2.41
150 10 – 0.00 2.26 1.75 2.48
200 10 – 0.00 2.29 2.20 2.56
50 10 1M 0.00 1.74 2.23 2.11
100 10 1M 0.00 2.95 3.65 3.14
150 10 1M 0.00 3.02 4.10 3.88
200 10 1M 0.00 3.22 4.37 4.25
4 M.D. Hoang et al. / Construction and Building Materials 259 (2020) 119779

Table 3
Dissolution ability of SiO2 and Al2O3 after autoclave curing.

Curing regimes NaOH conc. add. Dissolution ratio, % of


P, MPa T, °C s, h Red mud Fly ash
SiO2 Al2O3 SiO2 Al2O3
0.4 144 10 – 0.34 3.87 1.94 5.22
0.8 170 10 – 1.05 5.65 6.75 8.25
1.2 188 10 – 2.18 7.22 7.58 13.65
1.6 201 10 – 2.25 8.12 8.18 16.58
1.2 188 4 – 1.46 5.74 6.86 8.69
1.2 188 8 – 1.95 6.25 7.08 11.88
1.2 188 12 – 2.22 7.48 7.84 15.88
1.2 188 16 – 2.71 8.35 8.94 16.87
0.4 144 10 1M 1.28 4.25 8.34 6.25
0.8 170 10 1M 1.87 6.25 9.69 10.25
1.2 188 10 1M 2.38 7.98 11.65 16.35
1.6 201 10 1M 2.89 8.45 13.72 20.25
1.2 188 4 1M 1.95 6.42 10.33 10.33
1.2 188 8 1M 2.08 7.02 11.46 13.65
1.2 188 12 1M 2.44 8.33 13.00 17.98
1.2 188 16 1M 2.98 9.03 18.25 20.33

2.29% without addition of NaOH, and from 1.74% to 3.22% when the Further studies were carried out with a mixture of red mud
concentration of NaOH solution was 1 M. The corresponding values incorporating fly ash. High temperature curing regimes under
for fly ash were from 1.47% to 2.56% and from 2.11% to 4.25%, atmospheric pressure and properties of alkali activated materials
respectively. are shown in Table 4.
Under autoclave curing, the Al2O3 solubility of both red mud Red mud based alkali activated materials were only hardened
and fly ash were significantly improved. The solubility of Al2O3 under atmospheric pressure when it contained dissolved SiO2 by
improved with increasing pressure (and temperature) and dwell adding fly ash. The results in Table 4 show that with the same fly
time. In addition, in this condition, increasing the concentration ash content, raising the curing temperature from 50 °C to 200 °C
of NaOH solution also significantly increased the proportion of did not significantly increased the compressive strength of the
Al2O3 dissolved. The results showed that under autoclave curing, material. Without adding supplemental NaOH, available alkali in
the soluble Al2O3 content in fly ash and red mud could reach the red mud could also have activated the reaction. The compres-
20.33% and 9.03%, respectively. sive strength of material reached 6.9 MPa when cured at 200 °C
These results showed that it is possible to use the autoclave cur- for 10 h. However, the softening coefficient was relatively low (be-
ing to activate the components in the red mud to create a precon- low 0.46). The material was weakened in water saturated condi-
dition for synthesis of alkali activated materials. tions possibly due to the low degree of synthesis reaction or
geopolymerization and lack of cohesion. By adding NaOH, the
strength of the material was significantly improved, reaching
4. Influence of curing regime on properties of red mud based
9.6 MPa after 10 h of heating at 200 °C. The softening coefficient
alkali activated material
was also improved, but only to 0.57. This limitation impeded the
practical application of material, hence autoclave treatment should
Research on the effect of curing conditions on properties of
be applied to provide an additional active SiO2.
alkali activated materials was conducted with mixtures containing
Autoclave treatment of red mud and red mud-fly ash mixtures
only red mud and mixtures of which 26.3 wt% of red mud was
significantly improved the properties of material. When using red
replaced by fly ash. The liquid to solid ratio was chosen in accor-
mud without adding fly ash, we achieved the compressive strength
dance with the forming method and was equal to 0.2.
of 10.6 MPa with the softening coefficient 0.66 after 10 h autoclave
In this study, we also produced samples using only red mud
curing at pressure 1.6 MPa and temperature 201 °C. When we
(i.e., without adding fly ash) and curing at high temperature under
gradually added 1 M, 2 M, 3 M NaOH solutions, the strength did
atmospheric pressure. The samples were not hardened and lost
not change much but the softening coefficient was slightly
strength when soaking into water. This result is trivial and will
improved and reached 0.71. This observation showed that the syn-
not be discussed here. Again, this finding reconfirmed the fact that
thesis process took place by solely using red mud and there was no
the red mud itself does not have the ability to self-hardening under
need to have other component except mixing water. It is arguably
atmospheric pressure curing condition due to the absence of an
believed that the red mud based alkali activated materials can be
active SiO2.

Table 4
Properties of alkali activated material after high temperature curing.

Curing regimes NaOH conc. add. Rn, MPa Soft. coeff. pH Na2O residual, %
T, °C s, h
50 10 – 6.1 0.39 9.91 0.42
100 10 – 6.2 0.40 9.90 0.42
150 10 – 6.4 0.42 9.90 0.40
200 10 – 6.9 0.46 9.88 0.40
50 10 1M 9.0 0.51 10.40 0.51
100 10 1M 9.3 0.53 10.39 0.49
150 10 1M 9.6 0.56 10.38 0.48
200 10 1M 9.6 0.57 10.38 0.46
M.D. Hoang et al. / Construction and Building Materials 259 (2020) 119779 5

used as a building material in less water-affected areas. However, When adding 1 M NaOH, the material had a higher compressive
it is necessary to optimize the curing regime or add supplemental strength but, the leftover alkali increased to 0.38% (minimum value
active SiO2 to further improve the properties of the material. of 0.20%). However, the leftover alkali was still smaller than resid-
In our subsequent experiments, an active SiO2 was added by ual alkali after high temperature curing under atmospheric pres-
replacing 26.3% of red mud with fly ash. The autoclave curing sure condition. Similarly, the pH value of the material when
regime and the properties of the material are shown in Table 5. adding 1 M NaOH ranged from 9.5 to 9.8, but it was lower than
Experiments with the red mud – fly ash mixture showed that the pH of the material after high temperature curing (about 10.4).
the properties of the material were significantly improved. Raising Existing literature on geopolymer [5–9,26] and alkali activated
the pressure from 0.4 MPa (144 °C) to 1.6 MPa (201 °C), the com- material [10,17–19] shows the important role of a silicone dioxide
pressive strength of red mud-fly ash mixture without additional in forming structure and developing the strength of the material. In
NaOH increased from 7.4 MPa to 14.2 MPa after 10 h of dwell time. our experiment, while the total content of silicone dioxide was
Increasing dwell time also significantly improved compressive unchanged, the properties of the materials were varied depending
strength of the material. With a fixed pressure of 1.2 MPa on the curing regime. We suggest that only an active or dissolved
(188 °C), when we increased the curing time from 4 h to 16 h, silicone dioxide is contributing to synthesis of C-S-H, C-A-S-H,
the compressive strength raised from 11.0 MPa to 15.3 MPa. In C-N-A-S-H and geopolymer and affect the properties of the mate-
these experiments, the activation process was entirely based on rial. It means the regression between the content of the active sil-
leftover alkali in the red mud. After treatment, the residual Na2O icone dioxide and the properties of the materials can be
decreased significantly and not exceeded 0.23% (minimum value established.
of 0.14%) compared to 0.51% (minimum value of 0.40%) when cur- It is possible to calculate the total amount of dissolved SiO2 and
ing under atmospheric pressure conditions. The pH value of the Al2O3 as well as the ratio of two oxides for each mixture in each
alkali activated material after autoclave treatment was lowest at curing regime based on (i) the mixture proportion (73.7% red
8.99 compared with 9.88. mud and 26.3% fly ash), (ii) the content of dissolved SiO2 and
When NaOH is added, the properties of the material were Al2O3 in red mud and fly ash under the corresponding curing
improved. With the same curing regime, when adding 1 M NaOH, regime (Tables 2 and 3). Studying the correlation of these parame-
the compressive strength of the material varied from 11.3 MPa to ters with the properties of material shows that the active SiO2 con-
20.1 MPa (i.e. increased by 35% and 50%). However, the softening tent is closely correlated with the compressive strength. We also
coefficient did not change significantly as the NaOH concentration established the regression equations describing the relationship
increased. for the case of high temperature and autoclave curing by using
The softening coefficient linearly increased with dwell time and the least squares method (Fig. 2). The result showed that the com-
curing pressure (or curing temperature). In the water saturated pressive strength of the material is linear, co-variable with the con-
condition, the compressive strength of the material was reduced tent of dissolved SiO2 in the mixture.
in comparison with dry condition due to the additional stress that In our study, the ratio between the red mud and the fly ash were
occurred when the water penetrated into cracks and defects. fixed (we had a fixed SiO2/Al2O3 ratio of 0.93 in terms of total
Therefore, the softening coefficient also can be used to evaluate oxide). High temperature or autoclave curing did not change the
the defective degree of structure. Increment in the softening coef- ratio of the total oxide but only the ratio of the dissolved oxide.
ficient presented in Table 5 suggested that the structure of material The greater the amount of the dissolved SiO2 was, the more pro-
was less defective after autoclave treatment. According to [25], duct of synthesis reaction and the greater compressive strength
when the softening coefficient is greater than 0.85, the material of material was formed.
can be considered as water-resistant and can be used in wet areas. In Fig. 2, the content of the dissolved SiO2 after high tempera-
To produce a water-resistant alkali activated material, the red ture curing is relatively low, corresponding to the compressive
mud-fly ash mixture should be cured for 10 h and no less than strength is not exceeding 10 MPa. Autoclave curing promoted more
12 h under the pressure higher than 1.0 MPa (178 °C) and dissolved SiO2 up to 120 kg/m3 which significantly improved the
1.2 MPa (188 °C), respectively. With these curing conditions, the compressive strength. The combining regression equation for both
compressive strength of the material can be reached 10 MPa, curing regimes is as follow:
which is suitable to produce masonry unit. We recommend this
y ¼ 0:122  x þ 6:043 ð1Þ
curing condition for practical application.

Table 5
Properties of alkali activated material after autoclave curing.

Curing regimes NaOH conc. add. Rn, MPa Soft. coeff pH Na2O residual, %
P, MPa T, °C s, h
0.4 144 10 – 7.4 0.61 9.58 0.23
0.8 170 10 – 10.6 0.73 9.52 0.20
1.2 188 10 – 12.7 0.84 9.22 0.15
1.6 201 10 – 14.2 0.91 9.09 0.14
1.2 188 4 – 11.0 0.75 9.39 0.17
1.2 188 8 – 12.0 0.76 9.23 0.16
1.2 188 12 – 13.9 0.86 9.18 0.15
1.2 188 16 – 15.3 0.90 8.99 0.14
0.4 144 10 1M 11.3 0.62 9.75 0.35
0.8 170 10 1M 14.7 0.76 9.68 0.33
1.2 188 10 1M 17.4 0.85 9.58 0.23
1.6 201 10 1M 19.1 0.92 9.48 0.20
1.2 188 4 1M 15.2 0.76 9.59 0.30
1.2 188 8 1M 16.9 0.80 9.58 0.23
1.2 188 12 1M 18.7 0.86 9.56 0.22
1.2 188 16 1M 20.1 0.91 9.52 0.20
6 M.D. Hoang et al. / Construction and Building Materials 259 (2020) 119779

mud in ceramic materials production, Constr. Build. Mater. 163 (2018) 21–31,
https://doi.org/10.1016/j.conbuildmat.2017.12.092.
[2] M.P. Babisk, L.F. Amaral, L.S. Ribeiro, C.M.F. Vieira, U.S. Prado, M.C.B. Gadioli, M.
S. Oliveira, F.S. Luz, S.N. Monteiro, F.C.G. Filho, Evaluation and application of
sintered red mud and its incorporated clay ceramics as materials for building
construction, J. Mater. Res. Tech. 9 (2) (2020) 2186–2195, https://doi.org/
10.1016/j.jmrt.2019.12.049.
[3] A. Dass, S.K. Malhotra, Lime-stabilized red mud bricks, Mater. Struct. 23 (4)
(1990) 252–255, https://doi.org/10.1007/BF02472198.
[4] P. Krivenko, O. Kovalchuk, A. Pasko, T. Croymans, M. Hult, G. Lutter, N.
Vandevenne, S. Schreurs, W. Schroeyers, Development of alkali activated
cements and concrete mixture design with high volumes of red mud, Constr.
Build. Mater. 151 (2017) 819–826, https://doi.org/10.1016/
j.conbuildmat.2017.06.031.
[5] D. Dimas, I. Giannopoulou, D. Panias, Utilization of alumina red mud for
synthesis of inorganic polymeric materials, Miner. Process. Extr. Metall. Rev.
30 (3) (2009) 211–239, https://doi.org/10.1080/08827500802498199.
[6] J. He, J. Zhang, Y. Yu, G. Zhang, The strength and microstructure of two
geopolymers derived from metakaolin and red mud-fly ash admixture: a
comparative study, Constr. Build. Mater. 30 (2012) 80–91, https://doi.org/
10.1016/j.conbuildmat.2011.12.011.
Fig. 2. Effect of dissolved SiO2 content on compressive strength. [7] W. Hajjaji, S. Andrejkovičová, C. Zanelli, M. Alshaaer, M. Dondi, J.A. Labrincha,
F. Rocha, Composition and technological properties of geopolymers based on
Eq. (1) has R2 = 0.950, indicating a precise regression, which metakaolin and red mud, Mater. Des. 52 (2013) 648–654, https://doi.org/
10.1016/j.matdes.2013.05.058.
means that the regression between the compressive strength and [8] J. He, Synthesis and Characterization of Geopolymers for Infrastructural
the content of the dissolved SiO2 can be developed independently Applications. Doctoral dissertation Louisiana, State University, 2012, p. 105.
of the curing conditions. Based on that, Eq. (1) can be used to pre- [9] J. He, Y. Jie, J. Zhang, Y. Yu, G. Zhang, Synthesis and characterization of red mud
and rice husk ash-based geopolymer composites, Cem. Concr. Compos. 37
dict the compressive strength of the red mud and red mud-fly ash (2013) 108–118, https://doi.org/10.1016/j.cemconcomp.2012.11.010.
based alkali activated materials. [10] Z. Pan, D. Li, J. Yu, N. Yang, Properties and microstructure of the hardened
alkali-activated red mud–slag cementitious material, Cem. Concr. Res. 33 (9)
(2003) 1437–1441, https://doi.org/10.1016/S0008-8846(03)00093-0.
5. Conclusions [11] S. Smita, D.B. Rahul, M.U. Aswath, Experimental study on red mud based
geopolymer concrete with fly ash and GGBS in ambient temperature curing,
Int. J. Adv. Mech. Civ. Eng. 9 (2016) 5–8.
The curing regime had a great influence on synthesis as well as [12] A. Kumar, S. Kumar, Development of paving block from synergistic use of red
the properties of alkali activated material using red mud. Unlike mud and fly ash using geopolymerization, Constr. Build. Mater. 38 (2013) 865–
high temperature curing under atmospheric pressure, autoclave 871, https://doi.org/10.1016/j.conbuildmat.2012.09.013.
[13] M. Zhang, Geopolymer, Next Generation Sustainable Cementitious Materials -
curing made it possible to dissolve more SiO2 in red mud. The sol- Synthesis, Characterization and Modeling. Doctoral dissertation, Worcester
ubility of the oxides as well as the properties of the alkali activated Polytechnic Institute. 2015, p. 298.
material using red mud was significantly improved by increasing [14] M. Zhang, T. El-Korchi, G. Zhang, J. Liang, M. Tao, Synthesis factors affecting
mechanical properties, microstructure, and chemical composition of red mud–
curing pressure, dwell time and concentration of NaOH solution.
fly ash based geopolymers, Fuel 134 (2014) 315–325, https://doi.org/10.1016/
Red mud can be used independently or in combination with fly j.fuel.2014.05.058.
ash and NaOH to produce alkali activated material. Alkali activated [15] M. Zhang, M. Zhao, G. Zhang, J.M. Sietins, S. Granados-Focil, M.S. Pepi, Y. Xu, M.
Tao, Reaction kinetics of red mud-fly ash based geopolymers: effects of curing
material using red mud can achieve the compressive strengths up
temperature on chemical bonding, porosity, and mechanical strength, Cem.
to 10.6 MPa, the softening coefficient of 0.70. With the addition of Concr. Compos. 93 (2018) 175–185, https://doi.org/10.1016/j.
an active silica by replacing 26.3 wt% red mud with fly ash, the cemconcomp.2018.07.008.
compressive strength reached 20 MPa with the softening coeffi- [16] S.C. Choi, W.K. Lee, Effect of Fe2O3 on the physical property of geopolymer
paste, Adv. Mater. Res. 586 (2012) 126–129, https://doi.org/10.4028/
cient greater than 0.90. In addition, autoclave treatment under www.scientific.net/AMR.586.126.
high pressure and high temperature also reduced the residual [17] K. Sankar, P. Stynoski, G.K. Al-Chaar, W.M. Kriven, Sodium silicate activated
alkali and the pH of the material. Based on test result, the reason- slag-fly ash binders: Part I – processing, microstructure, and mechanical
properties, J. Am. Ceram. Soc. 101 (6) (2018) 2228–2244, https://doi.org/
able curing regime was proposed. 10.1111/jace.15391.
Autoclaved alkali activated material based on red mud or a mix- [18] K. Sankar, A. Sutrisno, W.M. Kriven, Slag-fly ash and slag-metakaolin binders:
ture of red mud and fly ash met the technical requirements and can Part II—properties of precursors and NMR study of poorly ordered phases, J.
Am. Ceram. Soc. 102 (6) (2019) 3204–3227, https://doi.org/
be used in the production of masonry units. 10.1111/jace.16224.
[19] K. Sankar, P. Stynoski, W.M. Kriven, Sodium silicate activated slag-fly ash
binders: Part III—composition of soft gel and calorimetry, J. Am. Ceram. Soc.
CRediT authorship contribution statement 102 (6) (2019) 3175–3190, https://doi.org/10.1111/jace.16219.
[20] Z. Zhang, H. Wang, J.L. Provis, A. Reid, Efflorescence: a critical challenge for
Minh Duc Hoang: Conceptualization, Methodology, Investiga- geopolymer applications?, in: Concrete Institute of Australia’s Biennial
National Conference, 2013.
tion, Writing - original draft, Writing - review & editing. Quang [21] G.L. Kalousek, Studies on the cementitious phases of autoclaved concrete
Minh Do: Validation, Resources. Van Quang Le: Investigation, Data products made of different raw materials, ACI J. Proc. 50 (1) (1954) 365–378.
curation. [22] W.M. Kriven, J.L. Bell, M. Gordon, Microstructure and microchemistry of fully-
reacted geopolymers and geopolymer matrix composites, Ceram. Trans. 153
(2003) 227–250.
Declaration of Competing Interest [23] E.N. Kani, A. Allahverdi, Effects of curing time and temperature on strength
development of inorganic polymeric binder based on natural pozzolan, J.
Mater. Sci. 44 (12) (2009) 3088–3097, https://doi.org/10.1007/s10853-009-
The authors declare that they have no known competing finan- 3411-1.
cial interests or personal relationships that could have appeared [24] B. Hanayneh, Influence of curing conditions on the properties of geopolymers
to influence the work reported in this paper. from untreated kaolinite, J. Am. Sci. 10 (3s) (2014) 42–49, https://doi.org/
10.7537/marsjas1003s14.06.
[25] The basic properties of building materials, in: H. Zhang (Ed.), Building
References Materials in Civil Engineering, Woodhead Publishing, 2011, p. 423.
https://doi.org/10.1533/9781845699567.7.
[26] J. Davidovits, Geopolymer Chemistry and Applications, 4th ed., Institut
[1] C. Scribot, W. Maherzi, M. Benzerzour, Y. Mamindy-Pajany, N. Abriak, A
Geopolymere, 2015, p. 644.
laboratory-scale experimental investigation on the reuse of a modified red

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