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Zhang 2018
Zhang 2018
h i g h l i g h t s
a r t i c l e i n f o a b s t r a c t
Article history: In this study, the effect of waste glass powder as a potential cementitious material on the strength, drying
Received 11 August 2017 shrinkage and sulfate attack resistance of slag mortar activated by the mixture of water glass and sodium
Received in revised form 22 May 2018 hydroxide was evaluated. Also, Central composite design and response surface method were used for the
Accepted 6 June 2018
optimisation of the alkali content (sodium oxide equivalent) and replacement ratio of waste glass powder
by maximising flexural and compressive strengths. The results of analysis of variance (ANOVA) indicated
that the accuracy of the developed strength models based on response surface method was satisfactory.
Keywords:
The optimal alkali content and replacement ratio of waste glass powder were found to be 8.31% and
Alkali activation cement
Response surface methodology
14.57%, respectively. Under this condition, the experimental values of 3-, 7- and 28-day flexural strengths
Optimization and 3-, 7- and 28-day compressive strengths of alkali-activated slag/glass powder mortar were 6.6 MPa,
Slag 7.1 MPa and 8.4 MPa, respectively and 49.2 MPa, 52.9 MPa and 66.4 MPa, respectively, which agreed clo-
Glass powder sely with the predicted values since the percentages of error were negligible in the range of 0–2.38%.
Strength When the alkali content was 8.31%, the addition of 14.57% waste glass powder in alkali-activated slag
Dry shrinkage mortar could improve the 3-, 7- and 28-day flexural and compressive strengths, reduce the dry shrinkage
Sulfate attack by up to 15.8% at 1 day and 20.3% at 120 days, and increase the resistance to sulfate attack.
Ó 2018 Elsevier Ltd. All rights reserved.
https://doi.org/10.1016/j.conbuildmat.2018.06.040
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
528 L. Zhang, Y. Yue / Construction and Building Materials 181 (2018) 527–534
effectively improved when glass powder is used as partial replace- recycling facility. Ordinary Portland cement (CEM I 42.5R) with a
ment of cement [20,21]. Blaine fineness of 368 m2/kg was used as the reference binder.
Glass powder (GP) is known to be rich in silica and it can be The chemical composition of these materials is listed in Table 1.
activated by alkaline media to form sodium silicate gel. Until Water glass had a chemical composition of SiO2 = 26% and
now, very limited studies have been conducted on alkali activation Na2O = 8% and the silicate modulus (MS) was 3.2. Sodium hydrox-
of glass powder or the mixtures of slag and glass powder. Chen ide (NaOH) and water glass were mixed to make MS (SiO2/Na2O)
et al. [22] found alkali-activated glass inorganic binders could value of 1.0 on the basis of the previous studies [12,31]. Activator
obtain high strength which was related to the activator and curing solution was prepared 1 day before the casting of mortars.
condition. Redden and Neithalath [23] reported that sodium Crushed limestone sand (density = 2.65 g/cm3, fineness modu-
hydroxide (NaOH)-activated glass powder binders could obtain lus = 2.4) was used as fine aggregate in all mortar specimens.
higher compressive strengths than the activated fly ash mixtures
at low heat curing temperatures, but the activated glass powder 2.2. Mix proportions and processing
binders suffered the higher strength loss under moist curing
conditions. Adding other materials, like slag or metakaolin, could 2.2.1. Response surface methodology
be better to control the strength loss. Torres et al. [24] showed that Response surface methodology (RSM) explores the relationships
the best 28-day strength was obtained at 27.7 MPa when the mix- between several explanatory variables and one or more response
ture of NaOH and sodium carbonate (Na2CO3) with 5% sodium variables and it comprises a group of statistical and mathematical
oxide (Na2O) was used to activate slag/waste glass (slag: waste techniques for model building and model exploitation [30,32,33].
glass = 70:30). The mechanical strength decreased with the RSM is useful for modeling and analyzing the problems in which
increase of the waste glass content. Furthermore, in alkali (NaOH a response of interest is influenced by several input variables with
or NaOH/Na2CO3)-activated slag/waste glass binders, the slag was the objective of optimizing this response [30,34].
the main contributor to strength at early ages and the contribution When RSM is used to find the functional relationship between
of waste glass to the strength development was only after 28 days the response and various factors, the most commonly used design
[25]. Avila-López et al. [26] studied the binders based on waste method is central composite design (CCD). A CCD is made orthog-
glass and limestone activated by NaOH/Na2CO3 with 9% Na2O. onal and rotatable by the choice of a, the axial distance from the
The results revealed that the highest 28-day strength was 38.8 design center. The value of a for rotatability is determined by the
MPa and the hydration products mainly included C-S-H, a silica number of points (nf) in the factorial portion of the design; in fact,
gel type phase, and crystalline phases such as pirssonite and gay- a = (nf)1/4. Therefore, the value of a for a design with two factors is
lussite. In addition, Wang et al. [27] studied the use of waste glass 1.414. Furthermore, for providing reasonably stable variance of the
sand (0%, 10% and 20%) instead of slag to prepare alkali- activated predicted response, the center runs must be included in the CCD.
mortar. NaOH and sodium silicate solution were used as activator. Generally, three to five center points are recommended. Fig. 1
The results showed that the slump increased with the alkaline shows the CCD for k = 2 factors [34].
solution (0.5%, 0.75%, 1%), the slump flow increased with the Additionally, in order to preserve the quality of the model, it is
replacement of glass sand and the compressive strength increased necessary to standardize the data with the coded variables. The
with the alkaline solution and glass sand replacement. values of these variables are in the range of 1 to 1. Eq. (1) is
These studies are mainly focused on NaOH or NaOH/Na2CO3 as employed to define the relationship between the coded values
activator to prepare alkali-activated binders based on glass or (xi) and real values (Zi).
slag/glass. However, the type of activator has great influence on
the strength of alkali-activated slag-based binders and the maxi- 2Zi ðZH þ ZL Þ
xi ¼ ð1Þ
mum strength can be achieved by using water glass solution ZH ZL
[3,28]. Considering utilization of waste glass, the objective of this
where xi is the value in coded variable, Zi is the real value, ZH is the
work was to study the feasibility of incorporating waste glass pow-
real value corresponding to 1 in coded variable, and ZL is the real
der as a potential cementitious material in combination with slag
value corresponding to 1 in coded variable.
to develop new binders activated with water glass. Response
In AAS cement, the alkali content in activator has large influ-
Surface Methodology (RSM) was used to determine the optimum
ence on mechanical properties, which finally affects shrinkage
mix-designed parameters (the alkali content and replacement ratio
[35–37]. Also, the amount of glass powder has apparent effect on
of glass powder) with maximum flexural and compressive
the strength of AAS mortar. When the amount of glass powder
strengths. Actually, RSM has been successfully applied in many
was more than 20%, the strength of AAS mortar began to decrease
areas, including physics, chemistry, biology, medical science and
[31]. Accordingly, two factors, namely Na2O equivalent (Na2O %)
sociology for the probabilistic evaluation of a system and concrete
(x1) and glass powder content(x2), were considered in alkali-
industry for the optimising parameters [29,30]. Based on the opti-
activated slag /glass powder (AASGP) mortar mix design and three
mum design parameters, the dry shrinkage and resistance to sul-
levels (6%, 8% and 10% for the Na2O equivalent; 10%, 15% and 20%
fate attack of alkali-activated slag/glass powder (AASGP) mortar
for the glass powder content) for each factor were chosen in refer-
were studied.
ence to existing study [15,21,31,38]. The coded variables and
corresponding real values were given in Table 2. As shown in
2. Materials and experimentation Eq. (2), a second order polynomial model was used to represent
the response(y) as a function of the independent variables.
2.1. Materials y ¼ b0 þ b1 x1 þ b2 x2 þ b3 x1 x2 þ b4 x1 2 þ b5 x2 2 ð2Þ
Commercially available slag was used. The specific gravity and where y is the predicted response; x1 and x2 are individual effects of
Blaine fineness of slag were 2.89 and 450 m2/kg, respectively. the Na2O equivalent and glass powder content, respectively; x1x2
The basicity coefficient Kb = (CaO + MgO)/(SiO2+Al2O3) was 1.06. shows the interaction effect between Na2O equivalent and glass
Glass powder (GP) with a Blaine fineness of 500 m2/kg was powder content; x21 and x22 are quadratic effects of Na2O equivalent
obtained by the grinding of cullet with various colors, from a glass and glass powder content, respectively; b0 is the constant; b1 and b2
L. Zhang, Y. Yue / Construction and Building Materials 181 (2018) 527–534 529
Table 1
Chemical compositions of slag, glass powder and OPC, wt%.
Table 3
Mix proportions of AASGP mortar suggested by central composite design.
Mixture code Na2O (%) Glass powder (%) Mixture proportioning (kg/m3)
Water glass NaOH Sand Slag Glass powder Water
1 8 15 180.29 41.97 1757.81 498.05 87.89 115.75
2 8 15 180.29 41.97 1757.81 498.05 87.89 115.75
3 10.83 15 244.07 56.82 1757.81 498.05 87.89 73.78
4 6 10 135.22 31.48 1757.81 527.34 58.59 145.40
5 6 20 135.22 31.48 1757.81 468.75 176.06 145.40
6 10 10 225.36 52.46 1757.81 527.34 58.59 86.09
7 8 22.07 180.29 41.97 1757.81 456.62 129.32 115.75
8 8 15 180.29 41.97 1757.81 498.05 87.89 115.75
9 10 20 225.36 52.46 1757.81 468.75 117.19 86.09
10 8 15 180.29 41.97 1757.81 498.05 87.89 115.75
11 8 15 180.29 41.97 1757.81 498.05 87.89 115.75
12 8 7.93 180.29 41.97 1757.81 539.47 46.46 115.75
13 5.17 15 116.51 27.12 1757.81 498.05 87.89 157.71
Table 4
Strength test results.
Table 5
ANOVA test results.
f 28f ¼ 5:75569 þ 2:87812x1 þ 0:26446x2 þ 0:0025x1 x2 Model p-value (Prob > F) and F-value obtained from ANOVA
result have the important influence on the evaluation of the
0:17406x1 0:00985x2
2 2
ð7Þ
selected model. The p-value (Prob > F) <0.05 indicates that the
selected model are statistically significant [41]. The p-values
f 3c ¼ 74:82629 þ 26:0881x1 þ 2:22990x2 0:025x1 x2
(Prob > F) from the f3f, f7f, f28f f3c, f7c and f28c models were all less
1:54781x1 2 0:07265x2 2 ð8Þ than 0.05, as shown in Table 5. It indicated that these strength pre-
dicted models were significant. Besides, if a regression model is
f 7c ¼ 64:8114 þ 25:05497x1 þ 2:01036x2 þ 0:0025x1 x2 statistically significant, the calculated F value must be greater than
the critical value of the F distribution [8]. The critical value can be
1:50344x1 2 0:07255x2 2 ð9Þ
obtained from the F distribution table, where F-tab = F0.05 (5,7) =
3.97. The calculated F values of f3f, f7f, f28f, f3c, f7c and f28c models
f 28c ¼ 75:65474 þ 27:98721x1 þ 3:11339x2
were 42.61, 27.48, 55.46, 113.56, 83.99 and 42.03, respectively.
þ 0:13250x1 x2 1:81094x1 2 0:12775x2 2 ð10Þ They are all greater than 3.97, and hence the F-values also implied
L. Zhang, Y. Yue / Construction and Building Materials 181 (2018) 527–534 531
the models were significant. The determination coefficients (R2) and for f28f model were 0.0005, <0.0001 and 0.0011, respectively,
from f3f, f7f, f28f, f3c, f7c and f28c models were 0.9682, 0.9515, which were all less than 0.05. However, x2 and x1x2 had no signif-
0.9754, 0.9878, 0.9836 and 0.9678, respectively. It meant that icant effect on the flexural strengths since the p-values were higher
there were only 3.18%, 4.85%, 2.46%, 1.22%, 1.64% and 3.22% varia- than 0.05. As seen in Table 5, the p-value of x21 was lower than x1
tions could not be respectively explained by f3f, f7f, f28f, f3c, f7c and and x22 for flexural strengths. This meant that its influence on the
f28c models. The high values of R2 suggested that the quadratic development of flexural strengths was highest. The order of the
models fitted very well into the experimental data. The lack-of- importance of the model terms for flexural strengths is x21, x1 and
fit p-values calculated from the f3f, f7f, f28f, f3c, f7c and f28c models x22. Similarly, for f3c, f7c and f28c, x1, x21, x2 and x22 were significant
were 0.2802, 0.5394, 0.5974, 0.1341, 0.5118 and 0.1314, respec- model terms and x1x2 did not have a significant effect. Moreover,
tively. The fitness of the models was evaluated through the lack x21, x1, x22 and x2 were significant in descending order.
of fit tests (p > 0.05), which indicated the selected models were
reliable and useful for prediction of the f3f, f7f, f28f, f3c, f7c and f28c 3.1.2. Response surface plots
[41,42]. The interaction effect between Na2O equivalent and glass pow-
When the p-value is less than 0.05, the model term indicates a der content on the flexural and compressive strengths is repre-
significant effect on the strengths. In the current case, x1, x21 and x22 sented by 3D response surface plots in Fig. 2. It was observed
were significant model terms for the flexural strengths, since the that each graph significantly decreased on both sides of the peak,
p-values for the f3f model were 0.0034, <0.0001 and 0.0489, respec- which indicated that the flexural and compressive strengths of
tively, for f7f model were 0.0256, <0.0001 and 0.0368, respectively, the AASGP mortars increased first and then decreased with the
Fig. 2. 3D response surface plots for the effects of Na2O equivalent and glass powder content on flexural and compressive strengths at the age of 3, 7 and 28 days.
532 L. Zhang, Y. Yue / Construction and Building Materials 181 (2018) 527–534
increase of Na2O equivalent and glass powder content. The low or of values of a desirability function (dj) is 0 dj 1, where 0 repre-
high alkali content was not good for the strengths of AASGP mortar sents an entirely undesirable response value and 1 shows an
and the ideal Na2O equivalent was in the range of 7%9%. When entirely desirable or ideal response value. By maximizing the
alkali content is low, the dissolution of aluminosilicate minerals geometric mean of the individual desirability functions, a multi-
and the release of Si ions in glass are low, and the amount of slag objective optimisation problem can be solved [44].
to be involved in the cementing reactions is limited. As a result, In this research work, the highest f3f, f7f, f28f, f3c, f7c and f28c were
it is difficult to form a dense microstructure, resulting in relatively the desirable mechanical properties for AASGP mortar. So it was
low strengths. However, excessive alkali content may increase dry necessary to maximise flexural and compressive strengths simulta-
shrinkage, which eventually lead to the decrease in the strengths neously. And these six responses (f3f, f7f, f28f, f3c, f7c and f28c) were
[22,37]. The addition of a suitable amount of glass powder to considered to be of equal importance. The solution of this multi-
AAS mortar had a positive effect on the strengths. In this study, objective optimization and its contour diagram are presented in
the strengths increased with the increase in glass powder content Fig. 3. The figures showed that, the optimal values of Na2O equiv-
up to about 15% but decreased when glass powder content alent (x1) and glass powder content (x2) with highest desirability of
exceeded this ratio. The fineness of glass powder is greater than 0.846 were 8.31% and 14.57%, respectively.
that of slag. When the glass powder content was less than 15%, The experimental flexural and compressive strengths of AASGP
the strengths were increased because of its filling effect. However, mortar with the optimum combination (8.31% Na2O +14.57% glass
when the glass powder content exceeded 15%, the strengths were powder) and the predicted values obtained from mathematical
decreased owing to the low activation of the glass by the alkaline equations are shown in the Table 6. The experiment was repeated
solution. Also the contribution of glass powder to strength devel- three times and the data given here were mean values. As shown in
opment is manifested only after 28 days [25]. Table 6, the percentages of error between measured and predicted
As shown in Fig. 2, the flexural and compressive strengths were values for the f3f, f7f, f28f, f3c, f7c and f28c were 0, 1.41%, 2.38%, 0.20%,
maximized when Na2O equivalent and glass powder content were 2.08% and 0.75%, respectively. They were all within the acceptable
controlled in a proper proportion. The contour line of the Na2O tolerance value of 10% according to China National Standard GB/
equivalent pattern was thicker and the three-dimensional pattern T17671. It proved that the verification experiments fitted well with
was steeper than the glass powder content pattern. This observa- the statistical predictions. For comparison, the strengths of AAS
tion suggested that the Na2O equivalent affected flexural and com- and OPC mortar also are reported in Table 6. AAS mortar had
pressive strengths more significantly than the glass powder higher strengths than OPC mortar. The optimised mixture exhib-
content, which was in accordance with the results from the vari- ited highest flexural and compressive strengths. Owing to the opti-
ance analysis of the established mathematical models. mum combination between Na2O equivalent and glass powder, the
f3f, f7f, f28f, f3c, f7c and f28c of AAS mortar were increased by 11.9%,
3.2. Optimization 14.5%, 10.5%, 15.0%, 8.2% and 9.8%, respectively.
Table 6
Experimental results of strength for AAS mortar, OPC mortar and optimised mixture.
Fig. 6. SEM images of AAS mortar and optimised mixture (left side AAS mortar and right side optimised mixture).
534 L. Zhang, Y. Yue / Construction and Building Materials 181 (2018) 527–534
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