Journal of Cleaner Production 383 (2023) 135439

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Journal of Cleaner Production

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

Development of high-strength geopolymers from red mud and blast

furnace slag
Umme Zakira a, *, Kai Zheng b, d, Ning Xie b, **, Bjorn Birgisson c
a
Zachry Department of Civil and Environmental Engineering, Texas A&M University, College Station, Texas, 77843-3136, USA
b
Shandong Provincial Key Laboratory of Preparation and Measurement of Building Materials, University of Jinan, Jinan, 250022, China
c
School of Environmental, Civil, Agricultural, and Mechanical Engineering, University of Georgia, Athens, Georgia, 30602, USA
d
Institute of Highway Engineering, RWTH Aachen University, Aachen, 52074, Germany

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

Handling Editor: Prof. Jiri Jaromir Klemeš The worldwide growing interest in green construction urges for innovation of building materials by reusing the
existing waste resources, especially industrial by-products like red mud, which has been an environmental
Keywords: concern in the last few decades. This paper presents a study that investigated the potential use of red mud as a
Waste reuse raw material in the development of high-strength geopolymers. A Sodium hydroxide (NaOH) and Sodium silicate
Red mud
(Na2SiO3) solution were used as the activation reagent for red mud, and blast furnace slag-derived geopolymers.
High-strength geopolymer
This study adopted two different mixing procedures while activating the raw ingredients. Additionally, Ten
Blast-furnace slag
Silica fume percent (10%) by weight silica fume was introduced as an additive to assess its impact on the formed geo­
Compressive strength polymers. The mechanical and microstructural properties of the geopolymers were characterized based on two
Microstructural characterization types of preparation processes. The synthesized geopolymers achieved extraordinary early compressive strength
as high as 68.8 MPa. A high proportion of red mud, 50 percent by weight, could be utilized as a raw ingredient
achieving a high strength of 66 MPa. The optimum initial molar ratios were reported based on the geopolymer
products’ compressive strength and microstructural performances. Silica fume was found to be an efficient ad­
ditive that enhanced overall performance, ensuring higher proportional use of red mud as a raw material.

1. Introduction applications, including its use as an environmentally friendly cementi­

Geopolymers are sustainable cementitious materials that have the
potential to replace ordinary Portland cement (OPC), which is respon­
sible for as much as 8% of the world’s carbon dioxide (CO2) emissions
(Andrew, 2018). Their performance is similar to that of OPC, but they
have the advantage of reclaiming industrial wastes as a source of
alumina silicate precursor resources (Hu et al., 2018). While
manufacturing hydraulic cement can cause from 600 kg to 1200 kg per
metric ton of carbon dioxide (CO2), depending on the efficiency of the
production and proportion of clinker (Y. Kim et al., 2018; Hanif et al.,
2017), the production of geopolymer cement results in carbon dioxide
(CO2) emissions ranging between 271 kg and 425 kg per metric ton
(Mclellan et al., 2011). In addition to being sustainable, geopolymers
have advantages over OPC in terms of strength, high-temperature
resistance, shrinkage, and acid resistance (Hu et al., 2019). The multi­
fold benefits of geopolymers unlock a notable range of possible
tious material.
The geopolymerization process involves the dissolution of alumino­
silicate oxides (Al3+ in IV-fold coordination) in alkali poly-silicate,
which yields polymeric Si–O–Al bonds and forms three-dimensional
semi-crystalline silico-aluminate structures. The general formula of the
silico aluminate structure is Mn[–(Si–O2)z–Al–O]n.wH2O, where M rep­
resents one or more alkali metals and z is the degree of polycondensation
or polymerization (1, 2, 3, or higher) (Davidovits et al., 1991; Davidovits
et al., 1994). There are three basic forms of geopolymers: poly(sialate),
poly(sialate-siloxo), and poly(sialate-disiloxo) with a Si/A1 of 1, 2, and
3, respectively (Davidovits et al., 1991). Davidovits et al. (1994) sug­
gested molar ratios of SiO2/M2O and SiO2/Al2O3 in the range of 4.0–6.6
and 5.5–6.5, respectively, for alkaline poly(sialate-disiloxo) with a Si/Al
of 3. A similar range of molar ratios, such as M2O/SiO2, 0.2–0.48,
SiO2/Al2O3, 3.3–4.5, and H2O/M2O, 10–25, was found suitable in other
studies (Khale and Chaudhary, 2007; Ye et al., 2016). Thus,

* Corresponding author.
** Corresponding author.
E-mail addresses: uz17@tamu.edu (U. Zakira), mse_xien@ujn.edu.cn (N. Xie).

https://doi.org/10.1016/j.jclepro.2022.135439
Received 22 December 2021; Received in revised form 22 November 2022; Accepted 28 November 2022
Available online 2 December 2022
0959-6526/© 2022 Elsevier Ltd. All rights reserved.
U. Zakira et al. Journal of Cleaner Production 383 (2023) 135439

geopolymerization needs an optimum molar proportion of alumina and there are limited studies on the effect of the mixing procedure and the
silicate, along with an alkaline medium, e.g., Na, K- hydroxide, a molar ratio of RM-based geopolymers. Moreover, compressive strength
Na2SiO3 solution that can serve as an alkali activator. Sodium silicate of 55 MPa or higher is designated as high-strength concrete by ACI
and sodium hydroxide solution are commonly used as the alkaline so­ 363R, 2010. In several research works, high-strength geopolymers have
lution, where OH− helps in the dissolution of Si4+ and Al3+ of the been produced with high calcium fine fly-ash-based mortar (Chindap­
feedstock, and Na+ contributes to the crystallization of the geopolymers rasirt et al., 2011), fly ash, and slag-based concrete (Neupane, 2018),
(Murayama et al., 2002). The sodium silicate to sodium hydroxide ratio yet, there are few studies on the development of high-strength geo­
plays a crucial role, as both low and high amounts of Na+ can impact polymers utilizing RM and industrial wastes.
compressive strength. Less Na+ and OH− impede complete dissolution This study aimed to develop high-strength geopolymers using RM.
and polymerization, and a high Na+ content weakens the geopolymer Waste materials, including RM and GGBS, were used as the source of
structure by leaving the excess Na+ residue in the sample (Rowles and alumina and silica, and sodium silicate and sodium hydroxide (NaOH)
O’Connor, 2003). Morsy et al. (2014) reported that the compressive solutions were used as alkaline reagents. The mechanical and micro­
strength of fly ash geopolymers increases as the sodium silicate to so­ structural performances of the RM- and GGBS-based geopolymers were
dium hydroxide ratio increases from 0.5 to 1.0, then decreases as the investigated by conducting a pH test, particle size analysis, x-ray fluo­
ratio decreases from 1 to 2.5. The aluminate silicate precursors of geo­ rescence (XRF), x-ray diffraction (XRD), scanning electron microscopy
polymers can be sourced from natural resources, e.g., metakaolin (SEM), and compressive strength tests. The effect of molar ratios and two
(Duxson et al., 2007), kaolinite (Xu and Van Deventer, 2003), and in­ different mixing procedures have been investigated based on the overall
dustrial by-products, such as fly ash (Jiang et al., 2020; Jiang et al., performances of the synthesized geopolymers. Silica fume was incor­
2020; Y. Wang et al., 2021), waste glass (Zhang et al., 2020; Xiao et al., porated into the optimized mixture to assess its impact on the me­
2020), slag (Xiao et al., 2021; S. Li et al., 2021) and soil waste (Capasso chanical and microstructural properties.
et al., 2020) and can be used effectively with varying alkaline dosages,
activation processes and curing conditions. 2. Materials and methods
Red mud (RM) or bauxite residue is a highly alkaline industrial waste
with an average pH of 11.3 ± 1.0 (Gräfe et al., 2011) that amounts to 2.1. Materials
about 55–65% of the processed bauxite ores in alumina refineries
(Paramguru et al., 2004). According to the US Geological Survey (Na­ Locally sourced RM (Chipin Group, Shandong, China) and
tional Minerals Information Center, 2020), 370 million metric tons of commercially available ground-granulated-blast-furnace slag (GGBS)
bauxite ores were mined globally in 2019, consequently expanding the (Gongyi Longze Water Purification Material Co., LTD) were used as raw
quantity of RM as a by-product to approximately 175 million tons materials for the geopolymer synthesis. The RM was air-dried and pul­
annually. China generates 70 million tons of alumina every year, which verized in a jaw crusher and oven-dried at 80 ◦ C for 12 h before being
represents more than half of the alumina produced globally and results ball-milled at 260 rpm for 3 min clockwise and another 3 min counter-
in an annual output of more than 70 million tons of RM. As massive clockwise. It was then passed through a No. 60 sieve (250 μm) to ensure
quantities of RM cannot be used effectively, China has a stockpile of its homogeneity and fineness. The alkaline reagent was made with
about 600 million tons that takes up large amounts of land and poses commercially available sodium hydroxide (NaOH) flakes (Sigma-
serious environmental risks (Zinoveev et al., 2021; Agrawal et al., 2022). Aldrich Co.) and water glass (WG) (Jiashan Yurui Refractory Material
Currently, the most common practice of managing RM is depositing it in Co., LTD) with 44% (by weight) sodium silicate SiO2: Na2O: H2O = 3.4:
a tailing pond or a landfill, which raises environmental concerns due to 1: 5.6). Commercially available silica fume (SF) (Gongyi Longze Water
its causticity, space consumption, and possible groundwater pollution. Purification Material Co., LTD) was used in combination with RM and
This urges for development of strategies for utilizing and managing GGBS to add active silica to the system.
these wastes. Utilization of red mud in building materials can be a viable
management strategy that may significantly reduce or prevent the
2.2. Methods
storage of the red mud (Liu et al., 2014; Vigneshwaran et al., 2019,
2020; S. Wang et al., 2021). In such a way, the goal of obtaining sus­
The mix proportions of the RM, GGBS slag, sodium silicate, and
tainable and cleaner production of low-carbon construction materials
NaOH used in the geo-polymerization process for this study are provided
can be achieved with the reuse of red mud on a large scale. As RM
in Table 1. Different weight percentages of RM and GGBS were incor­
contains alumina (Al2O3), hematite (Fe2O3), silicates (SiO2), and alkali
porated, keeping the alkaline reagent constant. RM50-ASF was prepared
oxides (Na, Ca, K), it can potentially be used as a raw ingredient in the
by replacing 10-wt percent of the GGBS with silica fume to assess the
development of geopolymers. It typically contains a low percentage of
effect. Two methods were followed to prepare the samples. Method A
alumina and mostly non-reactive silica (Singh et al., 2018). Therefore, it
involved homogenous mixing of dry ingredients (RM, GGBS, and SF) at
is usually pretreated and mixed with additional sources of alumina and
1500 rpm for 30 s, then adding a NaOH solution and mixing for another
active silica such as fly ash, Ground Granulated Blast-furnace Slag
30 s. After a 15-s delay, 196 gm of the sodium silicate was added and
(GGBS), silica fume, rice husk, metakaolin (Ye et al., 2016; Singh et al.,
mixed for 15 s at 1500 rpm and 30 s at 3000 rpm. The ratio of anhydrate
2018; He et al., 2013; S. Li et al., 2018; Hu et al., 2018; Nie et al., 2016).
sodium silicate to sodium hydroxide and water to binder (w/b) was 1.6
Silica fume increases the reactivity of Al3+ in GGBS more effectively
than fly ash and increases the reactivity of Na+ in the alkali reagent (Lee
Table 1
et al., 2016). Calcined feedstocks, e.g., GGBS, fly ash, and metakaolin,
Mix proportions (wt%) used for red mud (RM)-based geopolymers.
contain high amounts of CaO and exhibit higher reactivity during geo­
polymerization than non-calcined ones and enhance microstructural Method Mix ID RM GGBS SF
and mechanical properties of geopolymers (Khale and Chaudhary, Method A RM10-AS 10 90 0
2007). The dissolution of RM or aluminosilicate sources plays a vital role RM30-AS 30 70 0
in the physical and mechanical performance of the final products (Lig­ RM50-AS 50 50 0
RM50-ASF 50 40 10
uori et al., 2017). Several pretreatment strategies have been suggested in RM70-AS 70 30 0
the previous research to activate relevant elements in RM by thermal RM90-AS 90 10 0
(Hairi et al., 2015; Ye et al., 2014), alkali-thermal (Ye et al., 2016), Method B RM50-BS 50 50 0
mechanical activation (Y. Li et al., 2019; Singh et al., 2018) or combi­ RM70-BS 70 30 0
RM90-BS 90 10 0
nation of them (Kumar et al., 2021; Hertel and Pontikes, 2020). Hence,

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 U. Zakira et al. Journal of Cleaner Production 383 (2023) 135439

and 0.26, respectively, for all the mix proportions in method A. In

preparation for NaOH solution, 55 gm of NaOH flakes were mixed in tap
water and cooled at room temperature to adjust 3.5M sodium silicate to
1.2M solution. In Method B, after the first mixing stage, the activator
solutions (solution of 10M NaOH and sodium silicate) were added all
together and mixed for 90 s at 1500 rpm. The ratio of sodium silicate to
sodium hydroxide solution and water to binder was 2.5 and 0.26,
respectively. The details of the mixing processes are shown in Fig. 1.
Specimens with dimensions of 40 mm × 40 mm x 40 mm were
prepared using oiled standard steel molds. The specimens were placed in
a standard curing chamber at 60 ◦ C ambient temperature. They were
then removed from the molds after 24 h of curing and continued to cure
at the same temperature. A Universal Testing Machine (CMT5504) was
used to conduct compressive strength tests after 3 days and 28 days of
curing, according to ASTM C39 (ASTM C39/C39M, 2003) or GBT
50107–2010 (GB/T 50107-2010, 2010) at a constant strain rate of 0.5%
strain rate per minute. The standard error values for compressive
strength were calculated based on 3 replicates of strength tests. The pH
of the RM solution was measured by inserting a pH meter into a solution
of 2 gm of RM and 20 ml of water. The density of the samples was
measured according to ASTM C188 (ASTM C188-16, 2009) and the
Fig. 2. Particle size distribution of red mud (RM) and ground granulated blast-
particle sizes were analyzed by an LS13320 laser particle size analyzer. furnace slag (GGBS).
Powder XRD patterns were collected from samples on a D8ADVANCE
diffractometer, and a JSM-7610F field-emission scanning electron mi­
croscope (SEM) was used to image the morphology of the samples. Table 2
Chemical constituents of red mud (RM), ground-granulated blast-furnace slag
3. Results and discussions (GGBS) and silica fume (SF), wt%.
Components RM GGBS SF
3.1. Physical and microstructural properties of raw materials Fe2O3 34.81 0.29 0.04
SiO2 12.94 34.11 98.08
3
The density and pH of the RM were found to be 2.94 g/cm and Na2O 10.92 0.75 –
10.32, respectively. The high pH in RM results from the presence of Al2O3 – 17.77 0.34
TiO2 5.41
alkali metals. The density of GGBS is similar to that of RM (2.99 g/cm3); – –
CaO 4.2 33.15 0.12
the d50 of RM is 17.24 μm and of GGBS is 10.20 μm. The particles of the SO3 0.49 – 0.42
GGBS are finer than those of RM which have a larger surface area and P2O5 0.32 0.06 0.55
dissolve and react more rapidly in forming the geopolymer gel. Fig. 2 ZrO2 0.18 – –
shows the particle distribution of the raw materials. V2O5 0.16 – –
MgO 0.16 0.34
The X-ray fluorescence (XRF) results presented in Table 2 reveal that
–
K2O 0.14 – –
RM is rich in Fe2O3, SiO2, and alkali metals, but has no trace of Al2O3. MnO 0.1 – –
GGBS is rich in SiO2, Al2O3, and CaO, which indicates that it is a suitable Cr2O3 0.08 – –
supplement for the preparation of the geopolymer. Silica fume (SF) Cl 0.04 – –
contains SiO2 and a small number of other minerals. Both the XRD
pattern and XRF analysis results showed a similar chemical composition
3.2. Mechanical properties of geopolymer
of the raw materials (Fig. 3 and Table 2). According to Fig. 3, hematite
(Fe2O3) at 33◦ –37◦ (2θ), quartz (SiO2) at 22◦ (2θ), katoite (Ca2.93Al1.97
Table 3 shows the compressive strength of the geopolymers that were
Si0.64O2.56(OH)9.44) at 17◦ –18◦ (2θ) and calcite (CaCO3) at 29◦ (2θ) are
derived from RM and GGBS and activated with a NaOH and sodium
the major crystalline compounds present in the RM. Whereas, A broad
silicate solution. When the proportion of RM reduced, the compressive
bump distributed between 20◦ (2θ) and 36◦ (2θ) can be observed for
strength of the RM-GGBS-based geopolymers increased, except for the
GGBS indicating the existence of amorphous phases. The micrographs of
RM30-AS, which has a higher standard error than other mixtures. High
the RM and GGBS are presented in Fig. 4.
strength was achieved with the addition of up to 70% RM, by ACI 363R,
2010, as shown in Table 3.

Fig. 1. Details of mixing methods A and B used for red mud (RM)-based geopolymers.

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U. Zakira et al. Journal of Cleaner Production 383 (2023) 135439

Table 3
Compressive strength of red mud (RM)-based geopolymers.
Mix ID Initial molar ratio Compressive
Strength (MPa)

SiO2/ SiO2/ Na2O/ CaO/ 3d 28d

Al2O3 Na2O Al2O3 SiO2

RM10- 4.405 4.020 1.096 0.781 68.79 ± 68.62 ±

AS 5.91 1.99
RM30- 5.086 3.031 1.678 0.703 52.29 ± 60.44 ±
AS 6.57 8.03
RM50- 6.312 2.316 2.726 0.605 61.21 ± 65.70 ±
AS 2.02 2.02
RM50- 9.372 2.778 3.374 0.418 67.85 ± 67.29 ±
ASF 0.90 1.81
RM70- 9.172 1.774 5.171 0.479 45.97 ± 51.82 ±
AS 1.57 3.35
RM90- 23.472 1.349 17.395 0.309 12.05 ± 8.76 ±
AS 0.13 0.27
RM50- 4.974 2.164 2.299 0.768 19.06 ± n/a
BS 0.89
Fig. 3. XRD patterns of red mud (RM) and ground-granulated blast-furnace slag RM70- 6.942 1.557 4.459 0.633 14.33 ± n/a
(GGBS) (S, H, and C denote peaks of Tridymite, Hematite and calcite, BS 1.20
respectively). RM90- 16.782 1.100 15.259 0.433 3.99 ± n/a
BS 0.78

The initial molar ratios of Na2O/Al2O3 and SiO2/Al2O3 increased, N.B: n/a = not available (not tested).
and SiO2/Na2O and CaO/SiO2 decreased with the addition of the higher
amount of RM. High strength, up to 68.6 MPa, was achieved with RM-
and GGBS-based geopolymers. It is clear from Table 3 and Fig. 5 that the
compressive strength declined from geopolymers RM10-AS to RM90-AS,
correlating with the molar ratio of the elemental components of the raw
materials. Fig. 5 shows that the synthesized geopolymers attained 90%
and more of 28-day strength within 3 days of curing.
It is evident in Fig. 5 that a high strength of 65.7 MPa has been
achieved with Na2O/Al2O3 and SiO2/Al2O3 ratios of 2.7 and 6.3 when
50 wt percent of RM is incorporated. The addition of GGBS increases the
SiO2, Al2O3, and CaO content and maintains the balance of the molar
ratios. Fig. 6 shows that the addition of GGBS also increases the
compressive strength. The higher reactivity of GGBS accommodates
faster dissolution enabling the early formation of the geopolymer
network and subsequently high early strength, irrespective of alkaline
(Lee et al., 2016; Mohamed, Al Khattab, and Al Hawat 123AD). On the
other hand, with the diminution of the Na2SiO3/GGBS ratio, the strength
improves, as shown in Fig. 6. Based on the mechanical properties, the
RM50-AS allows the highest incorporation of RM and ensures high early,
as well as 28-day compressive strength. Therefore, RM50-AS is the
optimized mixture for developing high-strength geopolymers consid­
ering the maximum utilization of red mud.
The molar ratios of Na/Al and Si/Na play a vital role in the geo­
polymerization process as they denote the availability of Na+ ions for Fig. 5. Effect of initial molar ratio on compressive strength of red mud (RM)-
both dissolution and activation of aluminosilicates. After the based geopolymers.

Fig. 4. SEM micrographs of raw materials, (1) red mud (RM), and (2) ground granulated blast-furnace slag (GGBS).

4
U. Zakira et al.
Fig. 6. Effect of ground granulated blast-furnace slag (GGBS) and Na2SiO3/
GGBS ratio on compressive strength of red mud (RM)-based geopolymers.
aluminosilicates have been activated, the condensation process begins,
either between the Si4+ and Al3+ species, forming poly-sialate, or be­
tween the Si4+ ions, followed by the Al3+ ions and resulting in a rigid 3D
network of geopolymers. The former case occurs when the SiO2/Al2O3
ratio is low, and the latter case occurs when the SiO2/Al2O3 ratio is high
(Singh et al., 2018). An excess concentration of the Si4+ ion may hamper
the condensation process as happened in the RM90-AS sample in the
study. Thus, there is an optimal range of SiO2/Al2O3, SiO2/Na2O,
Na2O/Al2O3 that are suitable for geopolymer formation. Fig. 7 shows
that the optimum ratio of SiO2/Na2O is 3.25 based on the polynomial
interpretation. The compressive strength increases with a higher pro­
portion of GGBS and an increase in the SiO2/Na2O ratio, which agrees
with previous studies focused on slag-based geopolymerization (Tan
et al., 2020; Ali Shah et al., 2021). An increase of Si/Al ratio forms more
Si–O–Al bonds and results in an improvement in the compressive
strength (E. H. Kim and Leslie Struble, 2012). In contrast, the optimum
range for Na2O/Al2O3 and SiO2/Al2O3 is approximately 1.1–3.4 and
4.41 to 9.4, respectively. Ca/Si and Si/Al influence the strength of the
geopolymer significantly. In the current study, the optimum value of
Fig. 7. Effect of initial SiO2/Na2O on 28-day compressive strength of red mud
(RM)-based geopolymers towards determining optimum molar ratios with
polynomial correlation.
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Journal of Cleaner Production 383 (2023) 135439
CaO/SiO2 was found to be 0.64 for high strength RM- and GGBS-based
geopolymer as shown in Fig. 8. In summary, both a proper balance be­
tween the molar ratios and the method of mixing are key factors for
geopolymerization. The strength and molar ratios listed in Table 3
(Method B) prove the interdependency between the ion ratios; the
mixing procedure in method B might cause a hindrance in the conden­
sation process.
3.3. Microstructural properties of geopolymer
After 28 days of curing at 60 ◦ C, SEM was used to investigate the
morphological characteristics of geopolymers derived from RM and
GGBS. The micrographs of the geopolymers synthesized by Method A
and Method B are shown in Figs. 9 and 10, respectively.
Alkaline activation dissolves aluminosilicates, leading to the for­
mation of tetrahedral-shaped polymers and three-dimensional chain
networks that link the polymers. Compared to the SEM micrographs of
the raw materials shown in Fig. 4, the SEM images in Figs. 9 and 10 are
distinctly indicative of new phase formation. Geopolymer gels were
identified in all the samples, with a few partially reacted zones in be­
tween the unreacted minerals. The tetrahedral polymer can be seen in
the SEM images of geopolymers RM10-AS, and RM70-AS, and the gel
network formations are visible in the geopolymer RM90-AS. The geo­
polymers synthesized by Method A seemed to be denser, more con­
nected, and have fewer unreacted particles than those synthesized by
Method B. The tetrahedral polymers, unreacted minerals, and partially
reacted particles are visible in Fig. 10. The morphological structure of
RM50-BS was more compact than that of RM70-BS and RM90-BS, which
was also reflected by the compressive strength. The CaO content
increased upon calcination. The morphology of RM-90AS shows the gel
network initiation and is yet to be condensed same as the samples RM10-
AS to RM70-AS, which was subsequently echoed in the strength prop­
erties. The high CaO content in GGBS caused the formation of amor­
phous Ca–Al–Si gels during geopolymerization decreasing the
microstructural porosity and strengthening the geopolymers (Yip and
Van Deventer, 2003; Khale and Chaudhary, 2007).
The mineral phase characterization of the alkali-activated RM- and
GGBS-based geopolymers was performed by X-ray powder diffraction
(XRD) on powder samples that had been cured for 28 days. Figs. 11 and
12 depict the XRD patterns of geopolymers comprised of identical pro­
portions of the same raw materials that were prepared using Methods A
Fig. 8. Effect of initial CaO/SiO2 on 28-day compressive strength of red mud
(RM)-based geopolymers towards determining optimum molar ratios with
polynomial correlation.
U. Zakira et al.
Fig. 9. SEM micrographs of red mud (RM)-based geopolymers prepared by Method A and cured for 28 days: (a) RM10-AS, (b) RM30-AS, (c) RM50-AS, (d) RM50-
ASF, (e) RM70-AS, (f) RM90-AS.
Fig. 10. SEM micrographs of red mud (RM)-based geopolymers prepared by Method B and cured for 28 days: (a՛) RM50-BS, (b՛) RM70-BS, (c՛) RM90-BS.
and B, respectively. The large hump between 25o to 35o (2θ) in the XRD
pattern of the raw GGBS denotes the amorphous phase. In contrast, no
broad hump is visible in the raw RM samples; the major phases in RM are
hematite (Fe2O3) at 33◦ –37◦ (2θ), quartz (SiO2) at 22◦ (2θ), and calcite
(CaCO3) at 29◦ (2θ). There were distinct peaks in the geopolymers of
both sets of samples, and calcium silicate hydrate (CSH) was the major
reaction product in both. Previous studies found that calcium-rich
feedstock, e.g., blast furnace slag, produces a calcium silicate hydrate
(CSH) gel when activated with an alkaline solution (Khale and
Chaudhary, 2007). Fig. 11 shows that when the proportion of RM is less
than 50% (the ratio of RM to GGBS ratio is below 1:1), calcium
aluminum oxide hydrate appears and periclase (MgO) pyrophyllite
(Al4Si8O20(OH)4)0.33) and orientite (Ca2Mn3O10(OH)4 disappear. In
earlier studies, Yip and Van Deventer 2003 found that various types of
calcium silicate hydrate, calcium aluminate hydrate, calcium alumino­
silicate hydrate, and CSH are prevalent in high-weight percent GGBS
systems, and the calcium aluminum oxide hydrate (CA) phase enhances
the degree of polycondensation and leads to more micro-crosslinking
geopolymer networks that strengthen the geopolymers (Moudio et al.,
2021). The current study agrees with their findings. Pyrophyllite leaches
out Al3+ and Si4+ in an alkaline medium to form tetrahedral oligomeric
silicate or aluminate (Panda et al., 2018), and periclase, a
magnesium-rich phase, forms when there is an abundance of magnesium
in the geopolymer ingredients. Thus, a matrix with less than 50% RM
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Journal of Cleaner Production 383 (2023) 135439
has more calcium and alumina, is likely to form calcium aluminum oxide
hydrate and CSH after complete dissolution of pyrophyllite, and exhibits
enhanced mechanical strength. Fig. 12 shows that geopolymers devel­
oped by Method B possess five distinct peaks: calcium aluminum oxide
hydrate at 10◦ –12◦ (2θ), katoite (Ca2.93Al1.97Si0.64O2.56(OH)9.44) at
17◦ –18◦ (2θ), 32◦ –32.7◦ (2θ), and 44.4◦ –46◦ (2θ), pyrophyllite
(Al4Si8O20(OH)4)0.33) at 28.5◦ –29.3◦ (2θ) and orientite (Ca2M­
n3O10(OH)4. The geopolymers prepared with Method A did not form
katoite; rather a pyrophyllite peak was found in both of the geopolymers
made with Methods A and B. Katoite forms in a CaO–SiO2–Al2O3–H2O
system when the silica content is sufficiently low (Meller et al., 2005).
This observation reveals that due to more favorable geopolymerization,
more calcium, aluminum, and silicon-based phases were formed by the
Method A process than by the Method B process. The impact of this
phenomenon was proven by the higher compressive strength of the
geopolymers developed by Method A.
3.4. Effect of silica fume (SF) on RM-GGBS-based geopolymers
To assess the effects of silica fume on the microstructure and me­
chanical strength of RM-GGBS geopolymers, 10% of the GGBS in RM50-
AS was replaced with silica fume, which resulted in initial molar ratios
similar to those of the RM50-AS sample. The mix proportion was 50%
RM, 40% GGBS, and 10% silica fume, as shown in Table 1. The 28-day
U. Zakira et al. Journal of Cleaner Production 383 (2023) 135439

Fig. 11. XRD patterns of red mud (RM)-based geopolymers developed by Method A: CA, G, C, H, S, O, P, CSH, Py, and Pe denote peaks of calcium aluminum oxide
hydrate, gaultite, calcite, hematite, tridymite, orientite, potassium oxide nitrite, calcium silicate hydrate, pyrophyllite, and periclase, respectively.

Fig. 12. XRD patterns of red mud (RM)-based geopolymers developed by Method B: CA, G, C, H, S, O, P, CSH, Py, Pe, and K denote peaks of calcium aluminum oxide
hydrate, gaultite, calcite, hematite, tridymite, orientite, potassium oxide nitrite, calcium silicate hydrate, pyrophyllite, and periclase, katoite, respectively.

compressive strength of the sample with silica fume (Table 3), was highly dense microstructure of RM50-ASF. The X-ray powder diffraction
equivalent to that of the RM10-AS and RM50-AS samples. The early (XRD) analysis depicted in Figs. 11 and 13 illustrate that the mineral
strength of the RM50-ASF geopolymer was 10% greater than the geo­ phases of RM50-ASF are calcium aluminum oxide hydrate, gaultite
polymer without silica fume. The SEM images shown in Fig. 9 show the (Na4(Zn2Si7O18)(H2O)5), orientate (Ca2Mn3O10(OH)), hematite,

7
U. Zakira et al.
Fig. 13. Comparison of XRD patterns of geopolymers with 50% red mud (RM) with and without silica fume (SF): CA, G, C, H, S, O, P, CSH, Py, Pe, and K denote peaks
of calcium aluminum oxide hydrate, gaultite, calcite, hematite, tridymite, orientite, potassium oxide nitrite, calcium silicate hydrate, pyrophyllite, periclase, and
katoite, respectively.
tridymite, potassium oxide nitrite (K4O(NO2)2), and calcium silicate
hydrate. No pyrophyllite, periclase, or katoite were present in the RM50-
ASF geopolymer, which is identical to the geopolymers prepared with
10%RM (RM10-AS) and 30%RM (RM-30). The silica present in RM is
typically non-reactive (Singh et al., 2018), yet an additional source of
active silica needs to be incorporated to synthesize high-strength geo­
polymers. Silica fume increases the reactivity of alkali reagents, favor­
ably Na+ ions in the alkali reagents, and surges the reactivity of the slag
or GGBS by enhancing the reaction of Al3+ in GGBS (Lee et al., 2016). In
the current study, as shown in Fig. 13, the high reactivity of silica fume
and the presence of CaO in GGBS enabled the formation of calcium
aluminum oxide hydrate and C–S–H phases after the complete dissolu­
tion of pyrophyllite, resulting in a high-strength geopolymer that was
equivalent to the geopolymers with a lower proportion of RM, irre­
spective of the optimum range of the initial molar ratio.
4. Future recommendation
Although the mechanical properties of the alkali-activated RM show
a promising potential if combined with appropriate solid wastes and
activators, the life cycle assessment (LCA) of these RM-based cementi­
tious materials is imperative before the real practical applications.
Previous studies have demonstrated that sustainability takes three di­
mensions in the economic, social, and environmental domains (Ramos
and Abel, 2022); as a result, it is critical to assemble the knowledge and
bridge the research gaps that are relevant to the durability of solid waste
recycling from each of these three pillars to realize the alkali-activated
RM-based products and strategies. The potential sources resulting in
such complexities in the LCA study may include, but are not limited to,
the issues discussed as follows. First, the indirect implications in the
environmental footprint and cost, which raises the need to define the
boundaries and time scale of the analysis domain to select the appro­
priate temporal and spatial resolution for the LCA study. How to set up
the boundary of research to cover the major considerations in the LCA
8
Journal of Cleaner Production 383 (2023) 135439
framework is full of challenges. Second, the cost, performance, and
impacts of solid wastes can be localized or site-specific whereas the
current LCA typically adopts general values which simplified them.
Finally, the impact of the landfill and accumulation of solid wastes on
the environment and how they deteriorate the natural environment or
assets are barely understood. It is extremely hard to track the trace of
hazardous substances released from the landfilled solid wastes.
Furthermore, it is challenging to realize an accurate calculation due to
the lack of appropriate correlation between the laboratory testing data
and field performance data.
5. Conclusion
The potential use of industrial by-products and wastes in the devel­
opment of high-strength geopolymers was investigated in this study.
Two mixing methods were performed to activate the aluminosilicate
precursors, and silica fume was introduced as a highly efficient additive
in the geopolymerization of RM and the GGBS system. This study can
greatly contribute to the advantageous reuse of huge RM. The study
presents the mechanical and microstructural experimental testing re­
sults of RM- and GGBS-based geopolymers and drws the following
conclusions.
(1) The RM10-AS geopolymer, which was synthesized with 10% RM
and 90% GGBS, had the highest level of compressive strength:
68.8 MPa within 3 days by curing at 60 ◦ C ambient temperature
for an initial molar ratio of SiO2/Al2O3 = 4.41, SiO2/Na2O =
4.02, Na2O/Al2O3 = 1.1, and CaO/SiO2 = 0.78. However, RM50-
AS is the optimum geopolymer, based on the utilization of 50%
RM and achievement of a high strength of 65.7 MPa.
(2) Based on the polynomial fit, the optimum molar ratio of SiO2/
Na2O and CaO/SiO2 is 3.25 and 0.64, respectively. The optimum
range for Na2O/Al2O3 and SiO2/Al2O3 was found to be 1.1 to 3.4
and 4.41 to 9.4, respectively.
U. Zakira et al.
(3) The geopolymer samples prepared with premixing with NaOH
solution (Method A) showed better mechanical and microstruc­
tural performances than Method B where the NaOH and Na2SiO3
solution were introduced altogether. The geopolymers synthe­
sized by Method A were denser, more connected, and had fewer
unreacted particles than those prepared by Method B. The SEM
images showed that lower weight percent of RM in the raw in­
gredients resulted in geopolymer matrices that were more
condensed and compact, which also justified the strength results.
(4) With an RM to GGBS ratio below 1:1, XRD analysis showed that
the hydrated calcium-aluminum phase appeared and periclase
disappeared, which enhanced the mechanical strength. The
higher strength of the geopolymers developed by the Method A
was associated with enhanced Al3+-based aluminosilicate phase
formation; therefore, Method A was proven to be more efficient
than Method B
(5) Silica fume (SF) was proven to be an effective replacement for
GGBS, due to its increased reactivity that resulted in higher early
compressive strength. A high weight percent of RM with 10 wt
percent of SF was utilized and resulted in high strength of 67.3
MPa.
CRediT authorship contribution statement
Umme Zakira: Methodology, Data curation, Data interpretation,
Writing – original draft, reviewing, and editing. Kai Zheng: Methodol­
ogy, Data curation, Data interpretation. Ning Xie: Conceptualization,
Visualization, Supervision. Bjorn Birgisson: Conceptualization, Visu­
alization, Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgments
We would like to thank Jinmei Shi and Yuanchao Chen for their help
during the lab test.
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