Construction and Building Materials 179 (2018) 138–150

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Construction and Building Materials

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

Improvement of properties of architectural mortars prepared with 100%

recycled glass by CO2 curing
Ming-Zhi Guo a,b, Zhenjun Tu b,c, Chi Sun Poon b,⇑, Caijun Shi c
a
College of Mechanics and Materials, Hohai University, Nanjing 210098, PR China
b
Department of Civil and Environmental Engineering, The Hong Kong Polytechnic University, Hong Kong
c
College of Civil Engineering, Hunan University, Changsha 410082, PR China

h i g h l i g h t s

Addition of recycled glass in cement mortar impaired its mechanical properties.

CO2 curing enhanced compressive and flexural strength of recycled glass mortar.

CO2 curing contributed to decreased water absorption and porosity.

CO2 curing improved the microstructures (especially ITZ) of recycled glass mortar.

Porous structure facilitated deeper CO2 penetration and higher CO2 curing degree.

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

Article history: Previous studies have well demonstrated that recycled glass (RG) can be incorporated into cementitious
Received 3 January 2018 materials to replace 100% river sand as fine aggregates. However, this replacement was found to incur
Received in revised form 23 April 2018 adverse effects on the mechanical properties of the cement mortar. In this study, CO2 curing was
Accepted 23 May 2018
employed to ameliorate these drawbacks. The effect of CO2 curing on both of the mechanical properties
and microstructure of the RG incorporated cement mortar was studied by a series of laboratory tests. The
results showed that replacement of river sand by 100% RG led to a 37% decrease in compressive strength
Keywords:
and a 32% reduction in flexural strength of the mortar samples under conventional curing. Whereas, CO2
CO2 curing
Recycled glass
curing of these samples significantly enhanced both the compressive and flexural strength, with a more
Mechanical properties pronounced improvement on the former. Such improvements were further reflected by a decrease in
Microstructure improvement both the water absorption and porosity, and by an enhancement of the microstructure. This is attributed
to the fact that compared with the mortar samples prepared with 100% river sand, those prepared with
100% RG had a more porous structure due to the smooth surface of RG and thus a poor bonding between
the RG and the cement paste. However, such a porous structure encouraged CO2 gas to penetrate and dif-
fuse more easily into the cementitious matrix, resulting in a higher degree of CO2 curing.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction responsible for several improved properties of the cement mortar,

such as increased workability, enhanced resistance to chloride ion
In Hong Kong, about 300 tonnes of post-consumer waste glass penetration, and reduced drying shrinkage [4,7–10]. In addition,
bottles are generated every day. The majority of the waste glass the melting and re-solidification property of RG contributed to
is sent to landfills for disposal due to the lack of a glass manufac- enhanced mechanical properties when the glass mortars were sub-
turing industry in Hong Kong to serve as a viable recycling channel. ject to high temperature exposures [7,11]. More interestingly, the
To alleviate the burden on the landfills, the use of recycled glass decorative and aesthetic characteristic of different coloured RG
(RG) as an aggregate replacement material in concrete or mortar made the resulting products more aesthetically pleasing [1,4,7,12].
has been found to be an effective recycling option [1–6]. The However, the use of RG in cementitious materials is not without
near to zero porosity and non-hydroscopic nature of RG were limitations. The downside of a smooth surface was the normally
observed weak bonding between the RG and the cement paste.
As a result, concrete or mortar samples prepared with RG as aggre-
⇑ Corresponding author.
gates typically had higher porosities [2,13,14]. Also, the size and
E-mail address: cecspoon@polyu.edu.hk (C.S. Poon).

https://doi.org/10.1016/j.conbuildmat.2018.05.188
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 139

volume of voids in the interfacial transition zone (ITZ) of RG incor- was mainly mixed coloured (colourless, green and brown) and
porated cement products were larger than that in the correspond- was used as a full replacement (100%) of natural fine aggregate
ing river sand samples [15,16]. These drawbacks manifested by mass. Its specific gravity was 2490 kg/m3. The maximum parti-
themselves in inferior compressive and flexural strengths cle size of the GA was 5 mm, and the FM was 2.79. The typical par-
[1,7,8,17–19]. Such commonly observed disadvantages, to some ticle size distribution of the S and GA used in the experiment is
extent, limit a wider application of RG in the cementitious materi- shown in Fig. 1.
als. There is a need to address this problem to promote the use of
RG in the construction industry. 2.2. Mix proportions
It has been well known that CO2 curing can enhance the early
strength of cementitious materials [20–24]. During the CO2 curing The mix proportions (by weight) of the prepared cement mor-
process, calcium silicates in cement can react with CO2 rapidly tars using GA and S as fine aggregates are given in Table 2. For
to form calcium carbonates and calcium silicate hydrates all the mortar mixes, the total cement content was kept constant
[22,24–26], to produce high early strength. [27–29]. at 529 kg/m3, and the cement to aggregate ratio was kept at 1:3.
On the other hand, it has been found that concrete products The control mortar (S) was prepared with a constant water-to-
prepared by using RG as aggregates were prone to carbonation. cement (W/C) ratio of 0.51, and the W/C ratio of the GA mortar
Increasing the RG content was accompanied by an increase in the mixes was adjusted to 0.54 to provide a workability similar to that
carbonation depth [2,30–32]. For example, concrete prepared with of the control.
100% RG as fine aggregates experienced a 60% deeper carbonation
depth compared with those prepared with sand [2]. This is under- 2.3. Sample preparation
standable considering that RG incorporated concrete products nor-
mally had a higher porosity (as discussed above). Apparently, the A consistent mixing sequence and duration was adopted for the
more porous structure allows the CO2 gas to flow more easily preparation of the mortar samples. All the mortar mixtures were
and penetrate more deeply into the hydrated cement matrix. prepared in a standard rotating drum type mixer with a capacity
Therefore, a higher carbonation degree can be expected. Based on of 8 kg. Initially, cement and fine aggregates (S or GA) were mixed
the discussion above on the benefit of accelerated CO2 curing on for about 120 s at a low speed to attain a uniform dry mix. After
the early age mechanical properties of cementitious materials, this that, the required amount of water was gradually added, and the
perceived drawback provides a legitimate reason to employ accel- mixture was mixed thoroughly. Immediately after the mixing pro-
erated CO2 curing to ameliorate the poorer mechanical properties cess was completed, the workability of the freshly prepared mortar
of RG incorporated cementitious materials. was evaluated.
In this study, the effect of CO2 curing on the mechanical proper- For each mortar mixture, a total of twenty-four 40  40  160
ties and microstructure of the 100% RG incorporated cement mor- mm prisms were cast in steel moulds. All the samples were
tar samples was investigated and compared to the 100% river sand demoulded at 1 d after casting. Nine 40  40  160 mm prisms
incorporated counterparts. Changes in the compressive and flexu- were cured in water at a temperature of 25 ± 3 °C. After 3, 9, and
ral strengths were monitored. In addition, the corresponding alter- 28 d of curing, three prisms were removed from the water tank
nations in the microstructure, especially in the ITZ, was examined separately and tested for flexural and compressive strength. The
and correlated to the changes of the mechanical properties. The water absorption value was measured at the curing age of 28 d.
mechanisms behind the improved properties of the CO2 cured In parallel, nine 40  40  160 mm prisms were cured in a flow
mortars prepared by RG were also dissected. through CO2 chamber (described below) at a temperature of
25 ± 3 °C. After 1, 3, and 9 d of CO2 curing, three prisms were
2. Experimental programme removed from the chamber separately and tested for flexural and
compressive strength. Three additional 40  40  160 mm prisms
2.1. Materials
110.0
Cumulave percentage passing ( %)

100.0 GA S
The materials used to fabricate the architectural mortar were
cement, natural fine aggregate (Referred as S), and recycled fine 90.0
glass aggregate (Referred as GA). The cement used was an ordinary 80.0
Portland cement of strength class 52.5R (OPC, Green Island Cement 70.0
Limited, Hong Kong) complying with American Society of Testing 60.0
Materials (ASTM) Type I. Its chemical compositions and physical 50.0
properties are shown in Table 1. 40.0
The natural fine aggregate used in the sand-mortar mix was a 30.0
natural river sand (S) (mainly quartz sand), which was sourced
20.0
from the Pearl River. Its specific gravity was 2620 kg/m3. The
10.0
maximum particle size was 5 mm, and the fineness modulus
0.0
(FM) was 3.35.
5.00 2.36 1.18 0.60 0.30 0.15 0.00
The recycled fine glass (GA) was provided by a local glass bev-
BS Sieve Size (mm)
erage bottles recycler. It carried out the collection, washing, and
crushing processes of the waste beverage bottles. The GA used Fig. 1. Particle size distributions of fine aggregates.

Table 1
Chemical and physical properties of cement.

Constituents, % Physical properties

CaO SiO2 Al2O3 Fe2O3 MgO Na2O K2O SO3 L.O.I Specific gravity Fineness, cm2/g
63.15 19.61 7.32 3.32 2.14 0.13 0.32 2.03 2.34 3.16 3519
140 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150

Table 2
Mix proportions.

Mix notation Cement (kg/m3) Sand (kg/m3) Glass (kg/m3) water (kg/m3) W/C
GA 2.36–5
S 529 1588 0 0 271 0.51
GA 529 0 1588 0 284 0.54

were cured in the CO2 chamber for 9 d to measure the water First, the samples after the compressive strength test were
absorption values. crushed into small particles of less than 5.00 mm in size. After that,
the broken samples were oven dried at 105 °C for about 24 h to
2.4. CO2 curing method remove the free water, and then 50 g of the particle samples was
heated in a muffle furnace for 1 h at 520 °C and 950 °C, sequen-
A flow-through CO2 curing process was used to promote rapid tially. Generally, the mass loss between 520 °C and 950 °C is com-
strength development of the mortars. Fig. 2 shows the flow- monly related to the decomposition of calcium carbonate due to
through CO2 curing setup. The main body of the flow-through reac- the liberation of CO2 [35,36]. Therefore, the CO2 uptakes
tor was a PVC tube with an internal diameter of 150 mm and a (MCO2 ð%Þ) in the mortars can be determined by the Eq. (1):
length of 400 mm. CO2 gas of 100% purity was injected directly into M 520A^  C  M950A^  C
the chamber. The inlet flow of the CO2 gas was controlled by a flow MCO2 ð%Þ ¼  100 ð1Þ
M 105A^  C
controller to a rate of 1 ± 0.1 L/min.
where, M CO2 ð%Þ represents the CO2 uptake, %; M 105A^  C represents
2.5. Testing method the mass of the samples after 24 h of heating at 105 °C, [g]; M 520A^  C
represents the mass of the samples after heating at 520 °C, [g];
2.5.1. Flexural strength M 950A^  C represents the mass of the samples after heating at
A three point flexural strength test in conformity with ASTM C 950 °C, [g].
348 [33] was conducted at 1, 3, 9, and 28 d of curing age. The prism
specimens were tested in a universal testing machine (50 KN) 2.5.4. Phenolphthalein test
under a central line load while simply supported over a span of After the targeted age of CO2 curing, the samples were split into
120 mm. The specimens were then loaded at a displacement rate two halves, and a phenolphthalein alcohol solution (pH indicator)
of 0.20 mm/min until failure. The results reported are the average was sprayed onto the fractured surface to identify the extent of
of three specimens. the carbonation reaction. In the non-carbonated part of the speci-
men, where the samples were still highly alkaline, a purple-red
2.5.2. Equivalent compressive strength colouration was observed. In contrast, the carbonated area showed
The equivalent compressive strength test was carried out the original grey colour of the hydrated cement.
according to ASTM C 349 [34]. The compressive strength was
determined using a conventional compression with a load capacity 2.5.5. Permeable voids and water absorption
of 3000 kN on the broken pieces (portions of the prisms broken in The water porosity and water absorption test were conducted
the flexure strength test) at 1, 3, 9, and 28 d of curing age. The to assess the water permeability characteristics of the mortars in
reported test results are the average of six measurements. accordance with ASTM C 642 [37]. For this test, three 40  40 
160 mm prisms were cured in water for 28 d or CO2 for 9 d.
2.5.3. CO2 uptake First, the specimens were dried in an oven at a constant temper-
The CO2 uptake by the samples was determined by a furnace ature of 105 ± 5 °C until a constant weight was achieved (Wod).
heating method because the formed CO2 can be liberated by ther- Afterwards, the dried specimens were immersed in a water bath
mal decomposition of the carbonates in the specimens. (21 ± 2 °C). After 30 min and 96 h of water immersion, the

Fig. 2. Set-up of flow-through CO2 curing.

 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 141

specimens were removed from the water bath to evaluate the mass subjected to constant agitation for 24 h at 40 °C. The resulted solu-
gained to determine the initial surface absorption (ISA) and final tions were filtered and stored in sealed plastic bottles for charac-
water absorption (FWA) values, respectively. The ISA and FWA val- terization using an inductively coupled plasma-atomic emission
ues were determined by the following equations: spectrometry (ICP-AES, Perkin Elmer Optima 3300DV).
ISA ¼ ½ðW30min  Wod Þ=Wod   100 ð2Þ
3. Results
FWA ¼ ½ðW96h  Wod Þ=Wod   100 ð3Þ
3.1. Influence of RG on compressive strength
where, W30min is the mass of the specimen after 30 min of
immersion, [g]; W96min is the mass of the specimen after 96 h of
Fig. 3 shows the effect of using 100% RG glass as fine aggregate
immersion, [g].
on the compressive strength of the mortars. Compared with the
After the water immersion, the apparent mass of the sample in
samples prepared with river sand (S-N), the 100% RG incorporated
water (Wwat) was determined. The permeable voids in percentage
mortars (GA-N) suffered a reduction of 37%, 42%, and 37% in com-
are given below:
pressive strength at 3 d, 9 d, and 28 d of curing, respectively. This
Permeable voids ¼ ½ðW96h  Wod Þ= ðW96h  Wwat Þ  100 ð4Þ finding was in good agreement with that of some previous studies
[1,13,18,39,40]. As discussed previously, the adverse effect of RG
on the compressive strength was mainly attributed to the weak
2.5.6. Measurement of micro-hardness bonding between RG and the cement pastes due to the RG’s
Based on the ASTM E384-16 [38] testing method, a digital smooth surface [18,40–42].
Vickers micro-hardness indenter (HVX1000A, China) was used to After CO2 curing, however, all the samples displayed much
measure the micro-hardness of the bulk mortars and the ITZ higher compressive strength than their normally water cured
between the aggregates and the cement pastes. Before testing, counterparts at the same curing age. For example, the compressive
cubic mortar samples with a dimension of 40 mm was obtained strengths of S-C and GA-C were 123.0% and 149.2% respectively of
by sawing the 40  40  160 mm prisms. Then, one of the sides that of their water cured counterparts after 3 d curing. The
(the non-forming surface) was finely grinded and polished to meet improvement in compressive strength was mainly due to the
the experimental requirements of the digital micro-hardness tes- decrease in porosity and increase in density [43]. It is worth noting
ter. The micro-hardness of the ITZ between the aggregates and that the RG incorporated mortar (GA-C) commanded a higher
the cement pastes was determined and compared. The measured strength gain in comparison with the sand incorporated mortar
distance was up to 160 lm and at an average of 20 lm spacing (S-C) after CO2 curing (Table 3). The compressive strength of GA-
from the surface of the aggregates. Each reported value was the C after 1 d of CO2 curing even exceeded that of those after 3 d
average of five measurements. The test load of the Vickers tester water curing. And after 9 d of CO2 curing, GA-C had a compressive
was 10 g with a 10 s contact time. strength comparable to that of the water cured for 28 d. In con-
trast, the compressive strengths of S-C after 1 d and 9 d CO2 curing
2.5.7. SEM observations were respectively lower than that at 3 d and 28 d of water curing.
The microstructure and elemental analysis of the samples after
9 d of CO2 curing (S/GA-C) and 28 d of water curing (S/GA-N) were
investigated using scanning electron microscopy with energy dis- 60
GA-N GA-C
persive X-ray spectroscopy (SEM-EDX, JEOL Model JSM-6490). 55
Compressive strength (MPa)

S-N S-C
The samples were gold coated, and selected highly polished surface
50
were tested by EDX. The SEM was operated at an accelerating volt-
age of 20 kV with a probe current of 70–78 lA. 45

40
2.5.8. XRD analysis
The mineralogy of the crystalline phases in the samples after 9 d 35
of CO2 curing (S/GA-C) and 28 d of water curing (S/GA-N) was ana- 30
lyzed using a high resolution powdered X-ray diffractometer (XRD,
Rigaku SmartLab). The scanning range was from 10° to 65° 2h with 25
5° min1 speed duration at 45 kV and 200 mA. 20

15
2.5.9. Porosity and pore size distribution
1d 3d 9d 28d
The porosity and pore size distribution of the samples after 9 d Ages
of CO2 curing (S/GA-C) and 28 d of water curing (S/GA-N) was mea-
sured using a mercury intrusion porosimeter (MIP, Poresizer9320, Fig. 3. Effect of RG on the compressive strength of water and CO2-cured mortars at
different curing ages.
micromeritics, USA). The samples were crushed to 5–10 mm in
size, immersed in acetone for 30 d, and dried at 60 °C for 7 d before
test.
Table 3
Compressive strength ratios between CO2-cured mortars and water cured mortars
2.5.10. Calcium ion leachability of waste glass (Cx/Wy).
Since the soda-lime glass contains a small amount of CaO, it is of
Mix notation Ratio of compressive strength
great interest to investigate the calcium leachability of RG to see if
there exists a potential reaction between the leached calcium ion C1d/W3d C3d/W3d C9d/W3d

and the dissolved CO2. First, the recycled glass particles used were GA 119.1 149.2 174.4
grounded into an average particle size of 50 lm. Then, 5 g of the S 95.9 123.0 143.4

grounded glass powder was put in 100 mL of two different NaOH Note: Cx/Wy represents the ratio of compressive strength of samples after x d CO2
solutions (pH = 10.5 and 11, respectively). The mixtures were curing to that of samples after y d water curing. (x = 1, 3, or 9 d; y = 3 d).
142 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150

Overall, the results clearly demonstrated that compared with the 7.00
sand incorporated mortars, the RG incorporated mortars were
more amenable to undergoing accelerated CO2 curing, which 6.00
5.16

CO2 uptake (%)

resulted in higher compressive strength at the early age.
5.00
3.85
3.2. Influence of RG on flexural strength 4.00

3.00
Similarly, the incorporation of RG in the mortar samples
resulted in a decline in the flexural strength (Fig. 4). Compared 2.00
with S-N, GA-N suffered a reduction of 21.2%, 19.3%, and 32.3% in 1.06
flexural strength at 3 d, 9 d, and 28 d of water curing, respectively. 1.00 0.57
This finding was also in line with our previous study [13]. The
explanation for the observed reduction in compressive strength 0.00
also applies here. Besides, a weaker ITZ, resulting from the weak S-N S-C GA-N GA-C
bond between RG and the cement pastes and the more porous
Fig. 5. CO2 uptake of the water and CO2-cured samples at 9 d.
structure in the immediate vicinity of the RG aggregates, is an
additional and more important factor contributing to the weaker
strength [15,16,18,41,42]. detected both the originally present and CO2-induced carbonates
After subjected to CO2 curing, both S-C and GA-C displayed in the mortars. The original carbonates in S-N and GA-N after 28
improved flexural strength in comparison with their water cured d of water curing were 1.06% and 0.57%, respectively. As stated
counterparts. For example, after 3 d of CO2 curing, the flexural by a previous study [44], the originally present carbonates can
strengths of S-C and GA-C were 126.9% and 117.9% of that of their come from the raw materials or from the naturally carbonation
respective water cured counterparts. However, it should be process in the presence of atmosphere CO2.
pointed out that unlike the improvement in compressive strength, The above findings were furthered confirmed by the phenolph-
CO2 curing exerted a more obvious improvement on the flexural thalein test on the split surfaces of the CO2-cured samples at 1, 3,
strength of the cement-sand mortar samples (Table 4). This seem- and 9 d (Fig. 6). It can be clearly seen that almost the whole surface
ingly contradictory finding will be discussed and explained later in of S-C was pink except a very thin ring along the perimeter
the discussion section. (Fig. 6(a)). In stark contrast, more areas along the perimeter of

3.3. Influence of RG on mass gain

Fig. 5 shows the CO2 uptake of S-C and GA-C at 9 d of CO2 cur-
ing. The mass loss induced by heating treatment demonstrated
that GA-C displayed a higher CO2 uptake than S-C. It should be
pointed out that the CO2 uptake determined by this method

9.00
GA-N GA-C
8.00 S-N S-C
Flexual strength (MPa)

(a) S-C (1d) (b) GA-C (1d)

7.00

6.00

5.00

4.00

3.00
1d 3d 9d 28d
Ages (c) S-C (3d) (d) GA-C (3d)

Fig. 4. Effect of RG on the flexural strength of water and CO2-cured mortars at

different curing ages.

Table 4
Flexural strength ratios between CO2-cured mortars and water cured mortars
(FCx/FWy).

Mix notation Ratio of flexural strength

FC1d/FW3d FC3d/FW3d FC9d/FW3d
GA 96.8 117.9 118.8
S 122.6 126.9 146.7 (e) S-C (9d) (f) GA-C (9d)

Note: FCx/FWy represents the ratio of flexural strength of samples after x d CO2 Fig. 6. Phenolphthalein indicator tests on the freshly split surfaces of CO2-cured
curing to that of samples after y d water curing. (x = 1, 3, or 9 d; y = 3 d). samples at 1, 3, and 9 d.
 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 143

the split surface of GA-C became colourless after 1 d of CO2 curing observations that the RG incorporated mortars were more easily
(Fig. 6(b)). Further CO2 curing led to a bigger difference in the carbonated by the accelerated CO2 curing process.
depth of red colour between S-C and GA-C, especially at 3 d of
CO2 curing, demonstrating and corroborating the above mentioned
3.4. Influence of RG on hardened density

2600 Fig. 7 shows the effect of using 100% RG glass as fine aggregate
on the hardened density of the mortars. Incorporation of 100% RG
2360 in the mortars decreased the hardened density. Compared with
Hardened density (kg/m3)

2400 2327
S-N, GA-N experienced an approximate 15.3% reduction in the
hardened density. Such a decrease was attributed to the lower
2200 specific gravity of glass (2.49 g/cm3) compared with that of river
2033 sand (2.62 g/cm3) [17]. After CO2 curing for 9 d, however, all the
1972
2000 samples displayed much higher values of hardened density than
their water cured counterparts. The enhancement in the hardened
1800 density was due to the filling of pores by the carbonation. It should
also be noted that the hardened density of S-C and GA-C was 1.4%
1600 and 3.1% higher than that of their water cured counterparts at a
S-N S-C GA-N GA-C curing age of 28 d, respectively. Once again, the RG incorporated
mortars experienced a higher increase in the hardened density,
Fig. 7. Hardened density of 28 d water cured and 9 d CO2-cured samples.
which agreed well with the improvement in the compressive
strength.

25.0 ISA (30min) FWA (96h) Permeable voids

ISA and FWA and permeable

20.7 3.5. Influence of RG on permeable voids and water absorption

20.0 19.0 18.8

The effect of using 100% RG glass as fine aggregate on the initial

15.0 surface water absorption (ISA, within the first 30 min), final surface
voids (%)

11.7
water absorption (FWA, 96 h), and permeable voids of the mortars
10.0 7.9 8.4 7.6 7.6 8.4 is shown in Fig. 8. It can be observed that GA-N showed a lower ISA
6.0
4.8 value than S-N after 28 d of water curing. However, when the cur-
5.0 3.6
ing period was extended from 30 min to 96 h, the FWA value of S-N
and GA-N became almost the same. On the other hand, the addi-
0.0 tion of 100% RG slightly decreased the permeable voids. This was
S-N S-C GA-N GA-C
consistent with the previous studies [14,45,46]. The decrease in
Fig. 8. ISA, FWA and permeable voids of 28 d water cured and 9 d CO2-cured the permeable voids can be attributed to the near-zero water
samples. absorption nature of RG [40].

105
Vikers microhardness (HV0.01)

95 S-N

85
75
65
55
45
35
25
15
0 20 40 60 80 100 120 140 160
Distance from the surface of aggregate ( μm)

(a)
Vikers microhardness (HV0.01)

105
95 S-C

85
75
65
55
45
35
25
15
0 20 40 60 80 100 120 140 160
Distance from the surface of aggregate (μm)
(b)
Fig. 9. Vickers micro-hardness developments at ITZs of S-N at 28 d water curing (a) and S-C at 9 d CO2 curing (b).
144 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150

After 9 d of CO2 curing, however, all the samples displayed 800.0

Total Vikers microhardness (HV 0.01)

much lower values of ISA, FWA, and permeable voids. For example,

646.5
the ISA, FWA and permeable voids of S-C were 24.1%, 9.5%, and
8.2% lower than those of their water cured counterparts (S-N). Sim-
ilarly, the ISA, FWA, and permeable voids of GA-C were 52.6%, 600.0

451.5
42.9%, and 37.8% lower than those of their water cured counter-
parts. This was likely due to the decrease in porosity and increase

350.5
in density induced by CO2 curing [43]. It is worth noting that GA-C 400.0
had a higher decrease rate in ISA, FWA, and permeable voids com-

244.1
pared with S-C.

3.6. Influence of RG on micro-hardness 200.0

Fig. 9(a) shows the Vickers micro-hardness developments at the

ITZ of S-N at 28 d. The micro-hardness values in the 0  20 lm, 20 0.0
 100 lm, and 100  160 lm of the ITZs were approximately 25, S-N S-C GA-N GA-C
30, and 20, respectively. After 9 d of CO2 curing, the micro-
hardness values of S-C at 0, 20 lm, 40 lm, 60 lm, 80 lm, 100 Fig. 11. Total Vickers micro-hardness developments at ITZs of S-N and GA-N at 28 d
lm, 120 lm, 140 lm, and 160 lm from the surface of the aggre- of water curing and S-C and GA-C at 9 d of CO2 curing.

gates towards the cement pastes were 2.9, 0.3, 36.9, 30.9, 14.5,
80 lm, 100 lm, 120 lm, 140 lm, and 160 lm from the surface
29.1, 47.6, 38.0, and 7.3 respectively higher than those of their
of the aggregates towards the cement pastes were 48.3, 44.7,
28 d water cured counterparts (S-N) (Fig. 9(b)). Owing to the for-
24.9, 32.9, 39.2, 37.3, 30.7, 17.8, and 20.2 respectively higher than
mation of carbonation products, the development of the micro-
those of their 28d water cured counterparts (GA-N) (Fig. 10(b)).
hardness of the control cement-sand mortar after 9 d of CO2 curing
The total Vickers micro-hardness of S-N, S-C, GA-N, and GA-C in
was greater than that of their 28 d water cured counterparts [47].
the areas of 0–160 lm away from the surface of the river sand or
The results imply that the ITZ and the cement matrix were both
RG was measured (Fig. 11). The total micro-hardness of S-C and
enhanced as a result of CO2 curing, which was consistent with
GA-C after 9 d of CO2 curing was 184.9% and 184.5% respectively
the results of a previous study [48].
of that of their 28 d water cured counterparts (S-N and GA-N), indi-
Fig. 10(a) shows the Vickers micro-hardness development at
cating a significant enhancement in the ITZ as a result of CO2
the ITZ of GA-N at 28 d. It can be seen that the micro-hardness
curing.
value in the 0–20 lm, 20–100 lm, and 100–160 lm were in the
range of 25–35, 29–42, and 45, respectively. Furthermore, RG
with the size of less than 100 lm might have certain pozzolanic 3.7. SEM observations
activity, which could also improve the ITZ between the cement
matrix and the RG [49–52]. Similarly, after CO2 curing for 9 d, To further examine the influence of CO2 curing on the ITZ
the micro-hardness values of GA-C at 0, 20 lm, 40 lm, 60 lm, between the cement matrix and the river sand or RG, SEM imaging

105
Vikers microhardness (HV0.01)

95 GA-N

85
75
65
55
45
35
25
15
0 20 40 60 80 100 120 140 160
Distance from the surface of aggregate (μm)

(a)
Vikers microhardness (HV0.01)

105
95 GA-C

85
75
65
55
45
35
25
15
0 20 40 60 80 100 120 140 160
Distance from the surface of aggregate (μm)

(b)
Fig. 10. Vickers micro-hardness developments at ITZs of GA-N at 28 d of water curing (a) and GA-C at 9 d of CO2 curing (b).
 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 145

Natural sand
aggregate
Cement paste

ITZ
ITZ
Cement paste

Natural sand
aggregate

Cement paste Glass sand

aggregate

ITZ ITZ

Cement paste
Glass sand
aggregate

Fig. 12. SEM images of the ITZs of S-N (a) and GA-N (b) at 28 d of water curing and S-C (c) and GA-C (d) at 9 d of CO2 curing.

a c

Ettringite

C-S-H
Calcium Calcium
hydroxide carbonate

C-S-H

Calcium
carbonate

Ettringite

b d
Fig. 13. Typical SEM images of S-N (a) and GA-N (b) at 28 d of water curing and S-C (c) and GA-C (d) at 9 d of CO2 curing.

was conducted. It can be seen that the ITZ of S-N after 28 d of water became slightly denser due to the formation of carbonation prod-
curing showed a typical dense microstructure (Fig. 12(a)). But ucts. But smaller strip-like pores were still observed (Fig. 12(c)).
strip-like pores with the largest size of approximately 10 lm were The ITZ of GA-N after 28 d of water curing was more porous
observed [53]. When subjected to CO2 curing of 9 d, the ITZ of S-C than that of S-N sample (Fig. 12(b)). Bigger strip-like pores were
146 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150

present and the interfaces between RG and the cement matrix All these observations were consistent with the previously results
appeared more loosely bounded, reflecting a weaker bonding. that the incorporation of GA impaired the compressive strength
Moreover, the smooth surface of the RG glass can be clearly seen. and flexural strength of GA-N samples.

S-N S-C GA-N GA-C

(a) (b) (c) (d) (e) (f) (g)

10 15 20 25 30 35 40 45 50 55 60 65

2Theta

(a) (b)

(c) (d)
Fig. 14. XRD spectra of the hydrated samples of S-N and GA-N at 28 d and CO2-cured samples of S-C and GA-C at 9 d (Figure a–g are the corresponding enlarged areas in the
original XRD spectra).
 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 147

(e) (f)

(g)
Fig. 14 (continued)

In contrast, the ITZ of GA-C after 9 d of CO2 curing became much silicate hydrates and a low CO2 concentration (<3%) [57,58], indi-
denser (Fig. 12(d)). More importantly, the strip-like pores disap- cating the complexity of the carbonation reaction process.
peared. Therefore, compared with S-C, GA-C experienced a much
more improvement in the ITZ due to CO2 curing. The SEM observa-
tions corresponded well to the improvements in the mechanical 3.9. Porosity and pore size distribution
properties (except for the flexural strength, which will be further
discussed below). Fig. 15 shows the cumulative pore volume of both the S-N and
Fig. 13 shows the typical SEM images of both the water cured GA-N at a 28 d curing age and the CO2-cured samples (S-C and GA-
and CO2 cured samples prepared with both river sand and RG as C) at a 9 d CO2 curing age. The porosity of S-N, GA-N, S-C, and GA-C
the aggregates. It can be seen that there were a large amount of were 12.58%, 17.11%, 11.00%, and 15.09%, respectively. Here, a
needle like ettringite crystals and a small amount of well- higher porosity of GA-N in comparison with S-N was confirmed
crystallized Ca(OH)2 crystals in the pores of S-N and GA-N. In stark once again. And the reduction in the cumulative pore volume of
contrast, calcium carbonates, instead of these ettringite and Ca both S-C and GA-C after CO2 curing was obvious. For example,
(OH)2, were observed in the S-C and GA-C samples.
3.0
3.8. XRD analysis S-N
S-C
2.5
Cumulative Pore Area (m /g)

The XRD patterns of the hydrated samples of S-N and GA-N at GA-N
2

28 d and CO2-cured samples of S-C and GA-C at 9 d are provided GA-C

in Fig. 14. After 28 d of water curing, both S-N and GA-N displayed 2.0
typical CH peaks at 18.02°, 34.05°, 47.12°, and 50.78° [54]. How-
ever, C-S-H was not detected due to its amorphous nature. After 1.5
9 d of CO2 curing, both S-C and GA-C showed less pronounced
CH peaks (even disappeared). Meanwhile, calcite peaks at 23.07°, 1.0
29.38°, 39.4°, and 47.4° increased. Moreover, the peak at 32.5°,
which corresponds to two overlapping peaks of C2S and C3S, was 0.5
lower than that of their water cured counterparts, indicating that
C2S and C3S were reacted with CO2. For GA-C, there was a small
0.0
vaterite peak at 23.07°, and small aragonite peaks at 26.2° and
36.0° (#PDF 041-1475) [55]. However, the characteristic peak of
10000 1000 100 10
vaterite at 24.8° was not observed (Fig. 14(b)). For S-C, there was
Pore size Diameter (nm)
also a minor vaterite reflection at 23.07°, and a minor aragonite
peak at 36.0° and 45.9° (Fig. 14(f)) [56]. The presence of the vater- Fig. 15. Pore size distribution of water cured samples of S-N and GA-N at 28 d and
ite and aragonite can be attributed to the carbonation of calcium CO2-cured samples of S-C and GA-C at 9 d.
148 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150

of RG reacting with the diffused CO2 gas to form a considerable

0.08 S-N
Log Differential Intrusion (mL/g)

amount of carbonates in the RG incorporated mortars seems rather

S-C
0.07 low in an environment of negligible concentrations of Ca2+. It can
GA-N
GA-C be expected that there is a low possibility of surface etching of
0.06 RG under CO2 curing.
0.05
4. Discussion
0.04
Using RG as aggregate in construction materials represents a
0.03
sustainable option of recycling the waste materials in Hong Kong,
0.02 greatly alleviating the burden on the landfills. However, our
previous studies found that the down side of incorporating RG in
0.01 concrete or mortar was the commonly observed reduction in
0.00 mechanical properties, especially compressive and flexural
100000 10000 1000 100 10 strength, due to the weak bonding between the smooth surface
Pore size Diameter (nm) of RG and the cement pastes [1,7,17,19]. In this study, CO2 curing
was employed to address these drawbacks based on the rationale
Fig. 16. Log Differential Intrusion vs Pore size of water cured samples of S-N and that CO2 curing can boost the early strength of the cementitious
GA-N at 28 d and CO2-cured samples of S-C and GA-C at 9 d. materials because CO2 can react with calcium silicates in cement
rapidly to form calcium silicate hydrates and calcium carbonates,
and that the normally more porous structure of RG incorporated
the porosity of S-C and GA-C was 1.58% and 2.02% lower than that cementitious materials would facilitate deeper CO2 penetration
of S-N and GA-N, respectively, suggesting a higher CO2 curing and higher CO2 curing degree [20–26].
degree for the RG incorporated samples. The Log Differential Intru- The results well demonstrated that CO2 curing did contribute to
sion vs Pore size curves are shown in Fig. 16. It can be clearly seen an enhancement in both the compressive strength and flexural
that compared with S-N, GA-N had a higher content of pores larger strength of both the sand and RG incorporated samples (Figs. 3
than 180 nm. After 9 d of CO2 curing, both S-C and GA-C experi- and 4). Such improvements can be attributed to the filling of pores
enced a reduction in pore size to around 100 nm, and GA-C showed due to the rapid formation of cement hydrates and carbonates,
a greater reduction. resulting in a denser structure in the CO2 cured samples, which
were reflected by the enhanced hardened density (Fig. 7) and
reduced permeable voids and water absorption values (Fig. 8).
3.10. Potential dissolution of calcium ions from RG Furthermore, it should be pointed out that compared with S-C,
GA-C experienced a higher increase in compressive strength
Since the Ca-O bond (155 KJ/mol) is much weaker than the Si-O (Table 3) but a lower gain in flexural strength (Table 4). This seem-
bond (443 KJ/mol), there is high potential of Ca dissolution from ingly contradictory finding raised an interesting question of
the soda-lime glass [59]. When the dissolved Ca2+ meets the CO2 whether compressive strength is always linearly related to flexural
in the solution, they can combine and form carbonates, which strength as reported by previous studies [13]. For the compressive
could precipitate on the surface of the glass particles. To investi- strength, it is closely related with the porosity of the mortars. A
gate the carbonation potential of RG with CO2 gas, the dissolution denser sample normally has a higher compressive strength.
of calcium ions from RG was measured. Two pH values of 10.5 and Evidence from this study substantiated this hypothesis. It was
11.0 were chosen to simulate a CO2 curing environment since it observed that in comparison with S-C, GA-C absorbed more CO2
consumes calcium hydroxide and reduces the pH to less than 12. (Fig. 5), obtained a higher degree of CO2 curing (Fig. 6), experienced
The results showed that the dissolution of Ca ion from the RG a much improvement in the ITZ (Fig. 12), and gained a more pro-
was observed in an alkaline environment with the pH value of less nounced hardened density (Fig. 7). All such betterment translated
than 11.0 (Fig. 17). This was consistent with a previous study [60]. into a higher increase in compressive strength. However, the bond-
However, it should be noted that the concentration of Ca2+ dis- ing between the aggregate and the cement paste plays a predom-
solved was quite low at both pH values. Therefore, the possibility inant role in determining the flexural strength. River sand has a
coarser surface than RG. As a result, the bonding between the river
sand and the cement pastes is much stronger than that between
the smoother surface of RG and the cement pastes, which was
reflected by a superior flexural strength of S-N when compared
10
Ca concentration (mg/L)

to GA-N (Fig. 4). CO2 curing only led to rapid formation of cement
hydrates and the subsequent filling of pores, but failed to improve
8 the weak bonding between the RG and the cement pastes. This was
supported by a limited concentration of calcium ions released from
6 the RG (Fig. 17). Overall, CO2 curing failed to confer the RG incor-
porated mortars with a higher improvement in flexural strength
4 (Table 4). Therefore, caution should be taken when it comes to
interpretation of the relationship between compressive strength
2 and flexural strength in the glass incorporated cement mortars.
Alternative strategies have to be developed to make the RG
surface coarser to improve the bonding between the RG and the
0
pH=10.5 pH=11 cement pastes. Thus, future research in this regard is needed to
augment the flexural strength of the RG incorporated cementitious
Fig. 17. Ca ion dissolution of grounded RG in alkaline solutions. materials.
 M.-Z. Guo et al. / Construction and Building Materials 179 (2018) 138–150 149

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