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Construction and Building Materials 151 (2017) 1827

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Construction and Building Materials


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

Recycled glass as a supplementary filler material in spent coffee grounds


geopolymers
Arul Arulrajah a,, Teck-Ang Kua a, Suksun Horpibulsuk b,a,, Mehdi Mirzababaei c, Avirut Chinkulkijniwat d
a
Department of Civil and Construction Engineering, Swinburne University of Technology, Hawthorn, Victoria 3122, Australia
b
School of Civil Engineering and Center of Excellence in Innovation for Sustainable Infrastructure Development, Suranaree University of Technology, Nakhon Ratchasima
30000, Thailand
c
School of Engineering and Technology, Central Queensland University, 120 Spencer Street, Melbourne, Victoria 3000, Australia
d
School of Civil Engineering and Center of Excellence in Civil Engineering, Suranaree University of Technology, Nakhon Ratchasima 30000, Thailand

h i g h l i g h t s

 Recycled glass (RG) evaluated as a supplement to spent coffee ground (CG) geopolymers.
 RG provides mechanical and chemical strength supplementation to CG geopolymer.
 Heat-treated activated RG + CG geopolymers can achieve 10 MPa at 7-days compressive strength.

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

Article history: Recycled glass (RG) is a demolition waste, rich in silica and with a high shear strength and has been used
Received 26 April 2017 as a replacement material for sand in various construction applications. Spent coffee grounds (CG) is a
Received in revised form 6 June 2017 waste material derived from brewing coffee and has been recently studied as a recycled construction
Accepted 8 June 2017
material, due to its physical resemblance to sandy soils. Geopolymerization, is a green process which pro-
duces cementitious compounds using aluminosilicate-rich materials and alkaline liquids. In this research,
a new geopolymer construction material was produced using RG as a supplementary filler material to
Keywords:
stabilize CG. Fly ash (FA) and slag were used as the precursors to induce geopolymerization in this
Construction
Glass
new RG + CG construction product. To maximize the potential strength of the geopolymer, fine RG was
Coffee grounds added into geopolymer mixes in proportions of 25%, 50%, and 75% to observe the effects on the final
Geopolymer RG + CG product strength. The mixes were compressed into cylindrical specimens, cured at room temper-
Recycling ature (i.e., 21 C) and 50 C for 7 and 28 days, and tested for their unconfined compressive strength (UCS)
to observe the effect of the various RG replacement ratio on the strength of CG geopolymers. Scanning
electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDS) were used to further explain
the role of RG in influencing strength development. Higher RG contents were found to lead to higher UCS
values. A lower liquid-to-precursor (L/P) ratio was required to achieve a saturation point in strength
development. RG was found to provide mechanical strength and supplementary chemical bonding
strengths by dissolving and contributing Si+ ions to form geopolymeric substances.
2017 Elsevier Ltd. All rights reserved.

1. Introduction to hold liquid, and as a construction material in building facades,


doors and windows due to its transparent nature, which allows
Glass is an amorphous solid which constitutes largely of silica maximum sunlight into a building. Glass is an easily recyclable
(SiO2) [1]. It is widely used to make containers, beakers, and bottles product which can be crushed, melted and then remolded into var-
ious shapes and sizes [2]. However, currently large quantities of
used glass are either landfilled or stockpiled for future use because
Corresponding authors at: Department of Civil and Construction Engineering, current logistics and recasting technologies do not result in an eco-
Swinburne University of Technology, P.O Box 218, Hawthorn, Victoria 3122, nomical nor efficient glass recycling process [3]. On the other hand,
Australia (A. Arulrajah). School of Engineering, Suranaree University of Technology,
Nakhon Ratchasima 30000, Thailand (S. Horpibulsuk).
other wastes containing silica are widely recycled. For example,
E-mail addresses: aarulrajah@swin.edu.au (A. Arulrajah), suksun@g.sut.ac.th post-consumer glassware can be ground, mixed with foaming
(S. Horpibulsuk). agents, and heated to produce a porous foamed-glass which is

http://dx.doi.org/10.1016/j.conbuildmat.2017.06.050
0950-0618/ 2017 Elsevier Ltd. All rights reserved.
A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827 19

Table 1
Test plan for the strength assessment of RG + CG geopolymers.

Test type RG:CG:P (by dry mass) Na2SiO3: NaOH L/P (by mass) Curing temperature (C) Curing duration (days)
Modified proctor compaction 20RG:50CG:30FA 70:30 0.8, 1.0, 1.2, 1.4, 1.6 N/A N/A
35RG:35CG:30FA 70:30 0.4, 0.6, 0.8, 1.0, 1.2 N/A N/A
50RG:20CG:30FA 70:30 0.2, 0.4, 0.6, 0.8, 1.0 N/A N/A
20RG:50CG:30S 70:30 0.8, 1.0, 1.2, 1.4, 1.6 N/A N/A
35RG:35CG:30S 70:30 0.4, 0.6, 0.8, 1.0, 1.2 N/A N/A
50RG:20CG:30S 70:30 0.2, 0.4, 0.6, 0.8, 1.0 N/A N/A
UCS 20RG:50CG:30FA 70:30 0.8, 1.2, 1.6, 2.0 21, 50 7, 28
35RG:35CG:30FA 70:30 0.6, 1.0, 1.4, 1.8 21, 50 7, 28
50RG:20CG:30FA 70:30 0.4, 0.8, 1.2, 1.6 21, 50 7, 28
20RG:50CG:30S 70:30 0.8, 1.2, 1.6, 2.0 21, 50 7, 28
35RG:35CG:30S 70:30 0.6, 1.0, 1.4, 1.8 21, 50 7, 28
50RG:20CG:30S 70:30 0.4, 0.8, 1.2, 1.6 21, 50 7, 28

Fig. 1. SEM images of: (a) RG, (b) CG, (c) FA, and (d) Slag.

Table 2 (RG) in a number of construction activities. Medium and fine sized


Chemical composition of RG, FA, and Slag by XRF analysis. RG particles have been found to possess high shear strengths [7],
Chemical composition (%) RG CG FA Slag suitable for use as a recycled material in construction applications
SiO2 83.57 N.D. 75.45 35.21
such as embankment fills [8,9], masonry units [1012], and earth
Al2O3 2.43 N.D. 12.01 13.09 retaining structures [13]. Sand-sized RG can also be used as a fine
Fe2O3 0.86 4.13 3.96 0.45 aggregate, and has been previously bound with a fly ash geopoly-
CaO 12.53 32.15 2.72 43.55 mer to produce masonry units with a recorded 3-days UCS of
MgO N.D. N.D. N.D. 5.93
12 MPa [14]. Powdered RG was found to be a good pozzolan which
SO3 0.28 N.D. 0.78 0.85
K2O 0.33 45.31 2.97 0.92 may be used to potentially replace cement because of the large
TiO2 N.D. 18.41 N.D. N.D. total exposed surface which enables silica to be readily leached
by alkaline solutions [15,16]. However, the main concern with
N.D. = Not Detected.
using RG as a supplementary cementing agent or construction
material, is the alkali-silica reaction between the alkali found in
light-weight and possesses significant load-bearing strength [4]. concrete and alkaline activator liquids and the silica in RG.
Another example is silica fume, the by-product of silicon and Alkali-silica reaction is an expansive reaction which cracks con-
silicon-alloy manufacturing, is a waste product associated with cretes and reduces mortar durability, but using ground or pulver-
glass and is used as a supplementary cementing agent for concrete ized RG significantly minimizes the occurrence of alkali-silica
due to its high silica content [5]. reaction [17].
In Australia, approximately 1 million tons of waste glass is col- The aforementioned process, in which silica is leached by alka-
lected annually [6]. Crushed glass obtained from municipal and line solutions, is observed in the formation of geopolymers.
industrial sources in Australia is considered as a construction and Geopolymerization involves the breaking down of
demolition (C&D) waste [6] and can be reused as recycled glass aluminosilicate-rich materials by highly alkaline liquids to form
20 A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827

calcium silicate hydrate (CSH) [18] and aluminium-modified cal- distribution (PSD). Commercially available D-grade Na2SiO3 composed of 44.1% sili-
cic acid, sodium salt (1.6 < Molar Ratio  2.6) and 55.9% water, and reagent grade
cium silicate hydrate (CASH) gels [19]. The aluminosilicates, ter-
NaOH with 97% purity were used.
med as precursors (P) in the geopolymerization process, are RG and CG were the parent materials, which formed the bulk of the geopolymer.
industrial waste materials such as ashes from coal combustion RG was mixed with CG and Precursor at a CG:RG:P ratio of 50:20:30, 35:35:30, and
[20,21] and the burning of rice husk and sugar cane [22,23] which 20:50:30. Precursor was fixed at 30% as done previously to enable comparison
are rich in silica. Slag, a residue from refining iron, is rich in calcium between mixes with different RG ratios [44]. The P used in this experiment were
FA and Slag due to their efficiency in stabilizing other recycled construction mate-
oxide and silica is another precursor used in geopolymers. Like the
rial such as crushed brick [48] and C&D aggregates [49,50]. Two series of specimens
hydration of Portland cement, the formation of geopolymers were produced to contain either FA or Slag as their Precursor ratio. Sodium Silicate
results in the formation of cementitious compounds, which can (Na2SiO3) and Sodium Hydroxide (NaOH) were mixed for the alkaline liquid activa-
be used to bind loose aggregates into a strong composite material. tor (L) used to induce geopolymerization. A ratio of 70Na2SiO3:30NaOH was
adopted as this ratio was found in past studies to be very efficient [14,44,51].
However, unlike Portland cement, geopolymers are much greener
The dried granular solids comprising RG, CG and Precursor (FA or Slag) were
materials which produce zero carbon emissions [24]. Geopolymers mixed at the desired ratio until homogeneity in colouration could be observed. Con-
as alternative construction materials have increasingly garnered currently, the 70Na2SiO3:30NaOH mixture was prepared. The dried material was
the attention of researchers [2529] due to their low carbon foot- then mixed with L until an observable consistency was obtained. However, mixing
print. The popularity of geopolymers as alternative construction was limited to 10 min, particularly in Slag mixes, due to the high flocculation rate of
Slag geopolymers. Different L percentages were used, and the resultant mixes were
materials is also rising as civil engineers become increasingly
then subjected to modified Proctor compaction to obtain a maximum dry unit
aware of innovative alternative construction materials, which will weight versus L content curve to observe the influence of L on material compact-
promote a greener future [3034]. ness. With material density obtained from compaction results, specimens were
Spent coffee grounds (CG) is a granular, insoluble and highly statically compacted and reproduced in a 100 mm in height and 50 mm in diameter
split mold. These specimens were sealed in vinyl bags and cured at 21 C or 50 C.
organic waste derived from coffee brewing [35]. Coffee is one of
The curing durations were 728 days. UCS tests were then conducted on the spec-
the most popular beverages in the world [36], and estimations imens. Table 1 summarizes the material combination and test sequences used in
undertaken in 2007 reported that the world produced 7.2 million the UCS tests. Fragments obtained from the UCS tests were oven-dried for 24 h
tons of spent coffee ground [37]; while in 2015 the figure rose to and gold-coated to undergo scanning electron microscopy (SEM) and Energy-
8.6 million tons [38]. The highly organic CG is rich in nitrogen, dispersive X-ray spectroscopy (EDS) tests. SEM was conducted under 5 kV using a
Zeiss-SUPRA 40VP device. EDS was done at 20 kV using a peripheral INCA x-act
hence is commonly used as an agricultural fertiliser [39]. As
EDS instrument attached to the electron microscope.
most of the CG generated in the world is diverted to landfills,
CG was also studied for its effects as a leachate absorbent [40].
More recently, CG was studied as a source of biodiesel fuel
100.0
[41] and even reused as a supplementary food ingredient in bak-
ery products [42]. 90.0
Percentage Passing (%)

Due to the physical resemblance of CG with sandy soils, CG has 80.0


been evaluated as a construction material in embankment sub- 70.0
grades [4345]. These studies found that CG could indeed meet 60.0 RG
the structural strength requirements to be used as subgrade fill 50.0 CG
materials, but required proper treatment before becoming struc- 40.0 FA
turally adequate. Conventional soil stabilization methods employ- S
30.0
ing Portland cement and lime were found to be inefficient in 20.0
treating CG [45]. Fly ash (FA) and slag, wastes derived from the coal
10.0
combustion and iron mining industries respectively, were used as
0.0
precursors in CG geopolymers and achieved high compressive and 0.0 0.0 0.0 0.1 1.0 10.0
bearing strengths [44]. Particle Size (mm)
This research studied the effects of introducing RG as a supple-
mentary filler in CG geopolymers, with FA and Slag as precursors. Fig. 2. Particle size distribution of RG, CG, FA, and Slag.
The effects of different replacement ratios of RG on the geopolymer
density, optimum liquid content, and workability were evaluated
and analyzed. This research aims to further reinforce the usage of
green materials in infrastructure works by combining two tradi- 16.0
tional waste materials (RG and CG), into a valuable construction
material. Successful implementation of a recycled RG + CG material 15.0
Dry Unit Weight (kN/m)

as a construction fill material will furthermore reduce the demand 20RG:50CG:30FA


for increasingly scarce landfill space and provide an alternative 14.0
20RG:50CG:30S
solution for current waste management systems.
13.0
35RG:35CG:30FA

12.0
35RG:35CG:30S
2. Materials and methods
11.0 50RG:20CG:30FA
RG was sourced from a Construction and Demolition (C&D) waste recycling
plant in Melbourne, Australia. The RG was graded by the suppliers prior to collec- 10.0 50RG:20CG:30FA
tion, and was categorized as fine RG as all particles passed through the 4.75 mm
sieve. Fine RG was selected as it provides high shear strength compared to large-
sized RG. After procurement, RG was oven-dried at 100 C and then stored in air-
9.0
tight bags.
CG was sourced locally from cafes around Melbourne, Australia. CG was then 8.0
manually separated from other caf wastes such as teabags, serviettes, milk boxes
0.0 0.5 1.0 1.5 2.0
and capsules. The cleaned CG was then oven-dried at 50 C to avoid denaturing the L/P
highly organic particles [46]. Dried CG was then stored in air-tight bags for further
use. Commercially available FA and Slag from Australia were used. Sieve analysis Fig. 3. Modified Proctor compaction curve of CG geopolymers with different RG
was done on oven-dried RG according to ASTM [47] to determine its particle size replacement ratios.
A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827 21

3. Results and discussions range of L/P for RG + CG geopolymers to achieve maximum com-
paction is 0.21.6, which can be attributed to the porous CG being
SEM images captured on (a) RG, (b) CG, (c) FA, and (d) Slag in replaced by RG particles which have lower water absorbency. Also,
Fig. 1 shows that RG and Slag are polygonal, CG particles are porous increasing the ratio of RG in the geopolymer results in increased
and irregularly shaped, while FA particles are spherical. The XRF dry unit weight of the mix due to the significantly denser RG par-
results done on RG, FA, and Slag were summarized in Table 2. ticles, which replaces the lightweight CG. Moreover, due to
XRF analysis undertaken on the RG particles shows that it is dom- decreased microporosity with the inclusion of RG, the higher the
inantly composed of 83.57% of SiO2, with CaO being the second amount of RG, the lower the sensitivity of the mix towards
dominant compound at 12.53%. Theoretically, this means that the moisture variation. The maximum dry unit weight values recorded
inorganic compounds found in RG are conducive for geopolymer- by 20RG:50CG:30P specimens are 10.07 kN/m3 for FA and 11.12
ization as Si, Al, and Ca are required for the polymerization process kN/m3 for Slag, whereas the maximum dry unit weight values
to take place. Fig. 2 presents the particle size distribution of the recorded by 50RG:20CG:30P specimens are 13.87 kN/m3 for FA
materials used in the geopolymers and indicates that the RG and and 14.92 kN/m3 for Slag. Comparatively, the maximum dry unit
CG are sand-sized particles, with RG resembling coarse-grained weight of CG is 4.4 kN/m3 [35] and the maximum dry unit weight
sand and CG resembling medium-grained sand. On the other hand, of 70RG:30FA geopolymers is 18.1 kN/m3 [14].
FA and Slag fall into the particle size range of fine-grained soils Fig. 4 presents the 7-day UCS results of the RG + CG geopoly-
similar to silt. All the materials used were uniformly graded, but mers. Evidently, the UCS of CG geopolymers increases significantly
the fraction of smaller particles in RG is higher compared to the after the introduction of RG. Compared to CG + FA and CG + Slag
particle distribution of the other materials. Mixing RG and CG geopolymers, these supplemented geopolymers can easily gain
together with FA and Slag would increase the maximum dry unit compressive strengths of more than 1 MPa. At 7 days, geopolymers
weight with the finer FA and Slag particles filling in the voids at the dry side of the Optimum Liquid Content (OLC) are relatively
between the larger particles. inefficient, as the L/P ratio is too low to fully dissolve silica and alu-
Modified Proctor compaction tests done on the RG:CG:P mixes, mina to form cementitious compounds. At the wet side of OLC,
as shown in Fig. 3, indicate that with the increase of RG, the L con- most mixes develop UCSs exceeding 1 MPa, except for the RG
tent required to achieve maximum dry unit weight after com- + CG + FA mixes cured at 21 C. RG + CG + FA specimens cured at
paction decreases. Compared to CG geopolymers utilizing solely 50 C gain strength with the increase of L/P because elevated tem-
FA (L/P = 1.22.6) [43] or Slag (L/P = 1.52.5) [45], the optimum perature curing favors geopolymeric reactions in FA geopolymers

20RG:50CG:30FA, 7 Days 20RG:50CG:30S, 7 Days


3.0 3.0
2.5 2.5
UCS (MPa)

UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P L/P

35RG:35CG:30FA, 7 Days 35RG:35CG:30S, 7 Days


3.0 3.0
2.5 2.5
UCS (MPa)
UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P L/P

50RG:20CG:30FA, 7 Days 50RG:20CG:30S, 7 Days


12.0 12.0
10.0 10.0
UCS (MPa)

UCS (MPa)

8.0 8.0
6.0 6.0
4.0 4.0
2.0 2.0
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P L/P
21C 50C

Fig. 4. 7-days UCS of various CG + RG geopolymer mixes at different L/P ratios.


22 A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827

[52] as FA is high in silica content [53]. On the other hand, without geopolymers have saturation points in which the increase of L/P
catalyzation of geopolymeric reaction by heat treatment, the still may result in UCS increases, however, the increment is not
excess Al-Si precipitation in RG + CG + FA geopolymers hinders proportionate to the increase of L/P. These saturation points are
geopolymeric reactions by preventing contact between reactive 1.2, 1.0, and 1.2 for 20RG:50CG:30P, 35RG:35CG:30P, and
materials [54]. Furthermore, the oversaturation of liquid in 50RG:20CG:30P respectively regardless of precursors used. Com-
50RG:20CG:30P mixes at L/P = 1.6 renders heat treatment ineffec- pared to the OLC of these mixes, which are 0.4, 0.6, and 1.0 for
tive in preventing excess Al-Si precipitation. Hence, it is important 20RG:50CG:30P, 35RG:35CG:30P, and 50RG:20CG:30P respec-
for RG + CG geopolymers with FA as a precursor to be heat treated tively, the saturation points are situated at much higher L/P ratios.
for proper strength development. On the other hand, Slag speci- This indicates that for these geopolymers, a good balance between
mens do not show much variance in strength gain regardless of L/P is more important than the maximum compaction of the gran-
curing temperature, confirming that geopolymers with Slag as a ular solids, and that the geopolymeric bonds are the dominant con-
precursors can be cured adequately without elevated curing tem- tributors to UCS compared to the interparticle friction created from
peratures [55,56]. maximum material compactness. A balanced L/P ratio ensures that
Fig. 5 presents the 28-day UCS results of the RG + CG geopoly- the aluminosilicate in the mixes is fully utilized in the chemical
mers. The trend of strength development relative to the change reaction to produce desirable calcium silicate hydrate (CSH) and
in L/P is similar to that of the 7-day specimens. At 21 C, Slag aluminium-modified calcium silicate hydrate (CASH) gels required
geopolymers performed remarkably and developed UCS similar for geopolymerization [57,58].
to those cured at 50 C; with an FA precursor, the increase of L/P Generally, the UCS of RG + CG geopolymers increases with the
did not cause any significant variation in UCS. Mixes with high increase of RG in the mix. This can be attributed to the shear strength
L/P content have begun developing geopolymeric compounds in provided by RG particles [8]. Interestingly, 50RG:20CG:30S
contrast to the 7-days specimens, resulting in UCS values with specimens gain extremely high UCS values which exceed 10 MPa
lower L/P values. At 50 C, similar to the 7-day specimens, the at L/P > 1.2 after 7 days of curing. XRF results indicate that the Slag
UCS of 28-days specimens increases when L/P increases. However, used in this study has a dominant CaO composition of 43.55%.
as the geopolymeric reactions at 28-days had manifested, the OH- ions readily react with the abundant Ca (dissolved from CaO)

20RG:50CG:30FA, 28 Days 20RG:50CG:30S, 28 Days


3.0 3.0
2.5 2.5
UCS (MPa)

UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P L/P

35RG:35CG:30FA, 28 Days 35RG:35CG:30S, 28 Days


3.0 3.0
2.5 2.5
UCS (MPa)
UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P L/P

50RG:20CG:30FA, 28 Days 50RG:20CG:30S, 28 Days


12.0 12.0
10.0 10.0
UCS (MPa)

UCS (MPa)

8.0 8.0
6.0 6.0
4.0 4.0
2.0 2.0
0.0 0.0
0.0 1.0 2.0 3.0 0.0 1.0 2.0 3.0
L/P 21C 50C L/P

Fig. 5. 28-days UCS of various CG + RG geopolymer mixes at different L/P ratios.


A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827 23

to form CSH [28], enabling the mix to achieve high early (7 days) Fig. 7 shows the difference in the UCS of specimens cured for 7
strengths. This observation is consistent with findings by Ismail and 28 days using FA as a precursor. On the other hand, in Fig. 7 it
et al. [27]. The increased mechanical strength provided by RG parti- can be seen that Slag geopolymers develop high early strengths
cles, which possess a similar friction angle and shear strength as regardless of curing temperature. Only 20CG:50RG:30S specimens
compared to naturally occurring sand [59], and additional Si leached cured at 21 C at high L/P ratios show a significant difference in
from fine RG particles provided elevated compressive strength per- UCS between 7-day and 28-day. As explained earlier, Slag geopoly-
formance and supplemented the formation of geopolymers. mers gain early strength mainly by the formation of CSH, which is
Fig. 6 shows the difference in the UCS of specimens cured for 7 independent of the Si/Al ratio. However, at 20CG:50RG:30S the
and 28 days using FA as a precursor. Evidently FA geopolymers high amount of Si may start to hinder the geopolymerization pro-
cured at room temperature exhibits decrease in UCS when the cess due to excess unreacted compounds. This problem was not
L/P ratio goes beyond the optimum ratio. Alkaline activation causes present in 50 C -cured Slag geopolymers. On the other hand, com-
FA particles to dissolve and form NASH gels, which should merge paring all 7-day to 28-day UCS results show that the UCS of spec-
into larger masses with time [60]. However, due to excess Si in imens is increased or maintained after prolonged curing.
the mix which excessively increases the Si/Al ratio [61], and with- Interestingly, at low L/P values of 0.40.8, all geopolymers per-
out the help of elevated temperature curing, the process is hin- form relatively poorly, with UCS ranging from 500800 kPa. This is
dered as seen in Fig. 6. Moreover, the addition of Si-rich RG attributed to insufficient L content, which results in poor dissocia-
further increases the Si/Al ratio. Therefore, FA geopolymers cured tion of precursor material to form cementitious compounds,
at room temperature performed poorly at 7 days. However, there regardless of heat treatment or prolonged curing. After reaching
are large improvements in UCS after 28 days. With 50 C curing, the optimum L/P ratio, it is especially evident at 21 C curing that,
FA specimens develop higher overall UCS, and the difference Slag geopolymers outperform their FA counterparts. In short, FA
between the 7-day and 28-day specimens UCS was smaller. geopolymers require heat treatment to develop high UCS, whereas

20RG:50CG:30FA, 21C 20RG:50CG:30FA, 50C


3.0 3.0
2.5 2.5
UCS (MPa)

UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.8 1.2 1.6 2.0 0.8 1.2 1.6 2.0
L/P L/P

35RG:35CG:30FA, 21C 35RG:35CG:30FA, 50C


3.0 3.0
2.5 2.5
UCS (MPa)
UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.6 1.0 1.4 1.8 0.6 1.0 1.4 1.8
L/P L/P

50RG:20CG:30FA, 21C 50RG:20CG:30FA, 50C


12.0 12.0
10.0 10.0
UCS (MPa)

UCS (MPa)

8.0 8.0
6.0 6.0
4.0 4.0
2.0 2.0
0.0 0.0
0.4 0.8 1.2 1.6 0.4 0.8 1.2 1.6
L/P L/P
7-Days Curing 28-days Curing
Fig. 6. 7-days and 28-days UCS development of CG + RG geopolymers with FA as a precursor.
24 A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827

20RG:50CG:30S, 21C 20RG:50CG:30S, 50C


3.0 3.0
2.5 2.5

UCS (MPa)

UCS (MPa)
2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.8 1.2 1.6 2.0 0.8 1.2 1.6 2.0
L/P L/P

35RG:35CG:30S, 21C 35RG:35CG:30S, 50C


3.0 3.0
2.5 2.5

UCS (MPa)
UCS (MPa)

2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
0.6 1.0 1.4 1.8 0.6 1.0 1.4 1.8
L/P L/P

50RG:20CG:30S, 21C 50RG:20CG:30S, 50C


12.0 12.0
10.0 10.0
UCS (MPa)

UCS (MPa)

8.0 8.0
6.0 6.0
4.0 4.0
2.0 2.0
0.0 0.0
0.4 0.8 1.2 1.6 0.4 0.8 1.2 1.6
L/P L/P
7-Days Curing 28-days Curing
Fig. 7. 7-days and 28-days UCS development of CG + RG geopolymers with Slag as a precursor.

Table 3
Comparison of EDS results for 20RG:50CG:30P geopolymers cured for 7 days at different temperatures.

Element 20RG:50CG:30FA 7 days, 20RG:50CG:30FA 7 days, 20RG:50CG:30S 7 days, 20RG:50CG:30S 7 days,


21 C 50 C 21 C 50 C
Weight% Atomic% Weight% Atomic% Weight% Atomic% Weight% Atomic%
C 45.64 56.03 32.83 42.67 29.91 39.9 18.49 26.39
O 38.95 35.89 47.15 46.01 47.11 47.19 52.72 56.49
Na 2.3 1.48 4.16 2.82 6.13 4.27 6.5 4.85
Mg N.D. N.D. N.D. N.D. 0.66 0.43 1.03 0.73
Al 2.98 1.63 3.82 2.21 1.25 0.74 1.99 1.26
Si 8.25 4.33 9.89 5.5 8.69 4.96 11.16 6.81
K 0.54 0.2 0.64 0.25 0.57 0.23 0.55 0.24
Ca 0.89 0.33 0.97 0.38 5.7 2.28 7.55 3.23
Fe 0.45 0.12 0.54 0.15 N.D. N.D. N.D. N.D.

N.D. = Not Detected.

Slag geopolymers develop relatively high UCS values regardless of trace amount of iron, whereas Slag specimens contain trace
curing temperature. amounts of magnesium. From Table 3, the percentage of carbon
EDS was used to scan the geopolymeric bonds occurring in FA geopolymers was higher than Slag geopolymers. However,
within the RG + CG geopolymers. Table 3 compares the EDS at 50 C the percentage of carbon is significantly reduced.
results of 50CG:20RG:30P specimens cured for 7 days. The car- Sodium, Aluminium, Silica, and Calcium levels in the geopoly-
bon content represents CG: if the detectable percentage of car- meric compounds all show increase at 50 C curing, with the
bon is large, it indicates that the geopolymeric material is not increase more prominent in FA mixes, thus validating that ele-
effective in encapsulating the CG particles. FA specimens contain vated temperature curing aids the formation of geopolymeric
A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827 25

Table 4
Comparison of EDS results for CG:RG:Slag geopolymers with 20, 30, and 50% of RG.

Element 70CG:30S 7 days, 50 C 20RG:50CG:30S 7 days, 35RG:35CG:30S 7 days, 50RG:20CG:30S 7 days,


50 C 50 C 50 C
Weight% Atomic% Weight% Atomic% Weight% Atomic% Weight% Atomic%
C 29.91 39.9 18.49 26.39 15.87 23.15 11.66 18.94
O 47.11 47.19 52.72 56.49 52.18 57.15 46.8 55.46
Na 6.13 4.27 6.50 4.85 8.13 6.20 90 7.01
Mg 0.66 0.43 1.03 0.73 0.99 0.72 0.67 0.54
Al 1.25 0.74 1.99 1.26 1.48 0.96 2.44 1.76
Si 8.69 4.96 11.16 6.81 13.35 8.33 16.88 10.65
K 0.57 0.23 0.55 0.24 0.65 0.29 0.71 0.36
Ca 5.70 2.28 7.55 3.23 7.33 3.20 11.84 5.28
Fe N.D. N.D. N.D. N.D. N.D. N.D. N.D. N.D.

N.D. = Not Detected.

Element Weight% Atomic%

C 31.05 40.96
O 48.16 47.69
Na 5.19 3.58
Mg 0.78 0.51
Al 1.31 0.77
Si 6.84 3.86
K 0.3 0.12
Ca 6.38 2.52
(a)

Element Weight% Atomic%

C 24.86 34.16
O 49.7 51.27
Na 6.49 4.66
Mg 0.81 0.55
Al 1.62 0.99
Si 8.88 5.22
K 0.43 0.18
Ca 7.21 2.97
(b)

Element Weight% Atomic%

O 52.55 65.81
Na 10.46 9.12
Al 0.63 0.46
Si 30.11 21.48
K 0.28 0.15
Ca 5.97 2.98

(c)

Fig. 8. SEM of a 20RG:50CG:30 S specimen cured for 7 days at 21 C, and EDS results on (a) a large area of geopolymeric formation encompassing voids; (b) a smaller area of
relatively denser geopolymeric formation; and (c) an embedded RG particle.

substances. The levels of Na, Si and Ca are significantly higher in relies on the Al and Si whereas in Slag mixes, Ca and Si are
Slag geopolymers, indicating that the geopolymeric compound the main components in geopolymerization.
possesses a higher concentration of CSH and CASH gels. It can Table 4 shows that with the increase of RG in the dry material
also be deduced that the geopolymeric formation in FA mixes ratio, geopolymeric activities increase, as indicated by the increase
26 A. Arulrajah et al. / Construction and Building Materials 151 (2017) 1827

in Na, Si, and Ca and the decrease of carbon percentage in the provided mechanical strength to CG geopolymers due to high
geopolymeric formation. As shown in Table 4, a geopolymer with- inter-particle friction, but also supplemented the formation of
out RG consists of 8% of Si that it doubles to 16% when CG is geopolymeric substances by providing readily dissolvable Si into
replaced by 75% RG. Correlating the UCS and EDS results leads to the mix.
the inference that as RG increases, the resultant UCS of the mix L/P was an important parameter, which influenced strength
increases. development in these geopolymers. At low L/P ratios, insufficient
The SEM image of a Slag geopolymer specimen in Fig. 8 shows a alkaline liquid resulted in ineffective geopolymerization and
large polygonal particle cemented by geopolymeric substances. cementation, hence produced specimens with low UCS. By increas-
The corresponding EDS results show significant difference in Silica ing L/P, UCS increased until a saturation point was achieved. At sat-
concentration at (a) a large area of geopolymeric formation encom- uration point, RG supplemented CG + Slag geopolymers could
passing voids, (b) a smaller area of relatively denser geopolymeric easily achieve UCS values exceeding 1 MPa after 7 days of curing,
formation, and (c) an embedded particle. With the presence of regardless of a 21 C or 50 C curing environment. On the other
voids in the geopolymer in (a), exposed CG is prone to detection. hand, CG + FA specimens required heat treatment to achieve high
A concentrated scanning area as shown in (b) may better represent early UCS. The highest recorded UCS at 7 days was 10.86 MPa
the typical element ratio in a geopolymeric compound. The polyg- and corresponded with 20CG:50RG:30S at L/P = 1.2 cured at
onal particle in (c) does not contain carbon, and is largely com- 50 C. Conclusively, CG + Slag geopolymers were recommended
posed of Si and O. RG and Slag are both polygonal but due to the for use due to their independency on the elevated temperature
trace amount of detectable Ca, it can be deduced that the particle curing.
is RG. RG is a waste material abundantly available throughout the
From the EDS results, it can be inferred that a fractional amount world. This research indicated that the addition of RG into the
of RG dissolves and contributes to the formation of geopolymeric CG geopolymer mix would contribute to streamlining waste man-
substances, but large RG particles can be found to be cemented agement efforts, as large volumes of fill material are required
by the geopolymeric compounds. The RG used in this study has annually to construct roads and highways across the globe. A
particle sizes ranging from 0.075 mm to 4.5 mm, and fine RG par- green geopolymer encompassing the waste materials; RG CG,
ticles contain easily dissolvable Si which is highly pozzolanic [62]. FA, and Slag as an alternative construction material will indeed
In a past study, fine RG particles lesser than 0.1 mm were found to promote a sustainable future for the construction industry.
be effective pozzolans with properties similar to FA [63], whereas
another report considered RG finer than 0.3 mm to be an effective Acknowledgements
precursor for geopolymers [62]. 10% of the RG used in this study is
finer than 0.3 mm in diameter hence act to supplement the forma- The third author acknowledges the financial support from the
tion of geopolymeric substances, as shown in the difference of Si Thailand Research Fund under the TRF Senior Research Scholar
concentration in the geopolymeric formations with different per- program Grant No. RTA5980005 and Suranaree University of
centages of RG in Table 4. The embedded glass particle supports Technology.
past observations that in a RG geopolymer, the geopolymeric for-
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