Abstract
Cement has shaped the modern built environment, but its production generates substantial carbon dioxide emissions. Consequently, there is an urgent need to identify alternative cementitious building materials for sustainable construction. In this study, cement mortars (CMs) were produced by partially replacing cement with nanoclay (NC) and granite dust (GD). The replacement proportions (% by weight of cement) of these materials were 1.5, 3, and 4.5% for NC and 10, 20, and 30% for GD. For mortars containing NC but not GD, the strength was maximized when the NC replacement proportion was 3%. To evaluate the combined effect of partially replacing cement with both NC and GD on the fresh and hardening properties of cement-blended mortars, ternary binder mixtures containing 3% NC together with 10, 20, or 30% GD were prepared, and their workability, bulk density, compressive strength (at 7, 28, and 90 days), and flexural strength were measured. Increasing the content of NC and/or GD reduced the flowability of these mortars relative to that of the reference mortar mix because it increased the content of fine materials. CM containing 3% NC and 10% GD had the highest compressive strength at 7, 28, and 90 days while also having the greatest flexural strength when compared to the control mix. This is most likely due to the high silica and alumina content of NC and GD, as well as their high specific surface area, which would improve the maturity and density of the matrix when compared to cement alone.
1 Introduction
Because of the world’s growing population and the need for infrastructural development in many countries, global demand for and consumption of cement has increased significantly in recent decades. Unfortunately, cement production causes high emissions of carbon dioxide; consequently, there have been efforts to replace cement fully or partially with waste or supplementary cementitious materials that are rich in silica and alumina to meet sustainability targets and reduce greenhouse gas emissions. This has led to the emergence of new recycling strategies based on using waste materials such as granite dust (GD), fly ash, slags, or cement dust to partially replace cement and thereby reduce greenhouse gas emissions while also reducing the cost of producing cement mortars (CMs) by eliminating the cost of disposing of the used waste materials [1]. These strategies align well with the objective of reusing waste materials to reduce environmental pollution [2].
Nanotechnology is a new field of materials science and engineering with the potential to revolutionize concrete technology. Nanomaterials are materials with features or particle sizes on the order of a nanometer (10−9 m). The small size of these features and/or particles profoundly affects the properties of nanomaterials, giving rise to behaviors not seen in conventional materials. Among other things, nanomaterials have extremely high specific surface areas (SSAs). In CMs containing nanomaterials, nanoscale particles can fill voids and densify the interfacial transition zone [3,4], which can lead to beneficial improvements in strength and other physical properties important in construction materials [5].
Several different nanomaterials, including nano-SiO2, nano-Al2O3, nano-MgO, nano-CaCO3, nano-TiO2, and nano-ZrO2, have been incorporated into concretes and cement-based materials to improve their durability and mechanical properties [1,6,7,8,9]. One class of nanoscale additives that could be useful in this context is nanoclay (NC). NC is a general term for nanoparticles of layered mineral silicates, which can be classified into various groups depending on their chemical composition and morphology; the notable NC types include bentonites, kaolinite montmorillonite, hectorite, halloysite, and organically modified NC [10]. As a nano-pozzolanic material, NC reduces the pore size and porosity of the cement matrix while also improving the hardened properties of cement paste and mortar. It could therefore enable the creation of a wide range of high-performance cement nanocomposites [11], and several studies have shown that CMs containing the percentages of NC produced less permeable concrete, resulting in enhanced mechanical properties and durability performance compared to control mortar samples [6,12,13,14]. For example, Farzadnia et al. [15] reported that incorporating 3% halloysite NC into CMs increased the 28th day compressive strength by up to 24% relative to control samples. Similarly, Hakamy et al. [16] reported that adding montmorillonite NC to a reference cement paste reduced its porosity and water absorption by 31.2 and 34%, respectively, while increasing its density, compressive strength, flexural strength, fracture toughness, impact strength, and Rockwell hardness by 9.7, 40 and 42.9%, respectively. Finally, Chang et al. [17] found that adding nano-montmorillonite to cement paste improved some of its properties, especially its durability.
GD is a waste material that is formed in crusher units used to process rocks in quarries; it is widely available in Iraq. Several studies have examined the effects of using granite sludge waste as a cement replacement in mortar and concrete products. For example, Hamza et al. [18] fabricated concrete bricks using CMs containing up to 40% granite slurry by weight; the bricks with the most favorable physical properties were obtained using a mortar with a granite slurry content of 10%. However, it has also been reported that adding GD to CM reduces its workability [11].
Another study examined CMs in which the GD replacement percentage varied between 10 and 50% in 10% increments [19]. In this case, the mechanical properties of the mortar were most favorable with a GD replacement level of 30%; higher levels of GD replacement led to a reduction in strength. Studies on the production of colored masonry mortar indicated that up to 10% of the cement in mortar can be replaced with granite cutting waste without the loss of compressive strength [20]. Separately, it was found that replacing 5% of the cement in mortar with GD enhanced the mechanical properties and corrosion resistance of concrete [21] and that replacing up to 10% of the cement in a mortar mix with GD did not reduce the compressive strength of the subsequently prepared concrete [22]. Finally, a study on the use of marble and granite residues as sustainable cement replacement materials indicated that mixed mortars containing 5% of either material by weight could be viable alternatives to conventional cement [23]. Most of these studies suggest that the optimal replacement percentage of GD in CMs is in the range of 7.5–10% and that replacement at this level slightly reduces the concrete strength [24,25].
Although the addition of waste materials and nanoparticles to CMs has been studied separately, there has been little work on their combined use. In particular, little is known about the impact on the characteristics of concrete or CM when waste GD and NC are used together as high-surface-area powder additives. Therefore, experimental studies were conducted to evaluate the workability and mechanical properties of binary and ternary blended CMs in which cement is partially replaced with GD and NC. Significant environmental and economic benefits would be obtained if these materials could be recycled by using them to partially replace conventional cement binders in mortars or concretes without adverse effects on their physicochemical properties.
2 Materials and methods
All mortar mixes were prepared using type I ordinary Portland cement (OPC) satisfying the ASTM Standard C150-2004 [26]. The chemical composition and physical properties of this cement are presented in Tables 1 and 2.
Chemical composition of the cement and GD used in this work
| Oxide % (by weight) | |||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|
| Binder | CaO | SiO2 | Al2O3 | Fe2O3 | MgO | SO3 | Na2O | K2O | P2O5 | LF | LOI |
| Cement (OPC) | 64.40 | 20.18 | 5.23 | 3.34 | 1.80 | 2.98 | 0.07 | 0.44 | — | 0.96 | 2.71 |
| GD | 3.72 | 67.70 | 12.5 | 4.64 | 0.84 | 0.21 | 4.22 | 3.89 | 0.18 | — | 2.43 |
Physical properties of the cement and GD used in this work
| Property | Cement | GD |
|---|---|---|
| Specific gravity | 3.12 | 2.63 |
| Fineness (m2/kg) | 338 | 1,040 |
| Median particle size (µm) (d 50) | 16.8 | 12.8 |
| Strength and activity index (SAI) 7 days MPa | 100 | 62 |
| (SAI) 28 days MPa | 100 | 79 |
| Color | Grey | Off-white |
The NC used in this study was NC Cloisite Na+ supplied by Southern Clay Products, Gonzales, USA. The properties of this material given in the documentation provided by its supplier are presented in Table 3. The material was amorphous with a packed bulk density of 0.3356 g/cm3. Figure 1 shows a scanning electron micrograph of the NC, in which the agglomeration of NC particles is clearly visible. The mean particle size distribution of NC was 6.0 μm, as shown in Table 3.
Properties of the NC (Cloisite® Na+)
| Parameter | Values | Comments |
|---|---|---|
| Physical properties | ||
| Specific gravity | 2.86 g/cc | |
| Loss on ignition | 7.00% | |
| Particle size | ≤2.00 μm | 10% |
| ≤6.00 μm | 50% | |
| ≤13.0 μm | 90% | |
| pH | 10.12 | |
| Mechanical properties | ||
| Hardness, Shore D | 83 | 5% Cloisite®-reinforced Nylon 6 |
| Tensile strength, ultimate | 101 MPa | 5% Cloisite®-reinforced Nylon 6 |
| Elongation at break | 8.00% | 5% Cloisite®-reinforced Nylon 6 |
| Modulus of elasticity | 4.657 GPa | 5% Cloisite®-reinforced Nylon 6 |
| Flexural modulus | 3.78 GPa | 5% Cloisite®-reinforced Nylon 6 |
| Izod impact, notched | 0.270 J/cm | 5% Cloisite®-reinforced Nylon 6 |
| Thermal properties | ||
| Deflection temperature at 0.46 MPa (66 psi) | 96.0°C | 5% Cloisite®-reinforced Nylon 6 |
| Processing properties | ||
| Moisture content | ≤2.00% | |
| Descriptive properties | ||
| Modifier concentration (meq/100 g clay) | 92.6 | |
| X-ray diffraction d-spacing (001) | 11.7 Angstroms | |
| Color | Off-white | |
Scanning electron micrograph of Cloisite® Na+ NC layers.
The GD used in this study is a by-product of the granite processing industry. It was obtained from granite crushing and polishing sites in the Babylon governorate/industrial area as a moist solid with an approximate water content of 20%. The GD sludge received from the supplier was first dried at room temperature (25 ± 2°C) for 24 h to reduce its moisture content. It was then placed in an oven at 105°C until it reached a constant weight. Before use in mortars, the GD was ground in a ball mill (Los Angeles device) for 15 min to remove agglomerates, yielding a GD powder with the properties listed in Table 2. The chemical composition and physical properties of the GD powder are presented in Tables 1 and 2. A photograph and an SEM image of the GD powder are shown in Figure 2a and b, respectively, showing the irregular and angular appearance of the GD particles.
(a) GD powder. (b) Scanning electron micrograph of GD particles.
The specific gravity of OPC and GD is 3.12 and 2.63, respectively. Thus, the specific gravity of GD used is lower than that of cement (Table 3). Due to certain processes, the SSA of GD is higher than that of cement. The high SSA of the GD was determined to be 1,040 m2/kg, whereas that of OPC was 338 m2/kg. It is obvious that all the pozzolanic materials possess greater SSA than the OPC. The high SSA of the pozzolanic materials prepared for this study is a good presumption that they possess the right quality to potentially be an effective pozzolan. The GD particle size distribution ranges from 0.1 to 90 μm, respectively, with a mean diameter (d 50) of 12.8 μm. The pozzolanic activity of the raw GD was determined in accordance with ASTM Standard C311 (2006) [27].
The fine aggregate used to prepare the mortars examined in this work was natural river sand with a maximum grain size of 1.18 mm, complying with ASTM Standard C778-2002 [28]. The sand was obtained from the Alakader/Karbala governorate. The graded sand had a water absorption of 0.94%, a fineness modulus of 2.06, and a specific gravity of 2.59.
Table 4 shows the composition of the mortar mixes used in this study. The control CM was made using only OPC as the binder. Binary mortar mixes containing OPC and NC were prepared, in which NC replaced 1.5, 3, or 4.5% of the OPC by weight when compared to the CM. Binary mortar mixes containing OPC and GD were prepared, in which GD replaced 10, 20, or 30% of the OPC by weight. Finally, ternary mortar mixes were prepared, in which NC replaced 3% of the OPC by weight and GD replaced 10, 20, or 30% of the OPC by weight. Each mix is assigned a designation, in which the numbers preceding “NC” and “GD” indicate the replacement percentages of NC and GD, respectively. All of the mortar mixes had a binder content of 692 kg/m3 and a constant sand:binder (S/B) ratio of 1:2.25. The water:binder ratio (W/B) of all mortar mixes was also constant and was equal to 0.38. A modified polycarboxylic ether-based super-plasticizer (SP) sold commercially as Glenium 54 was added to all mortars at a concentration of 1.2% by volume to achieve the desired flowability. The SP, which was supplied as a whitish to straw-colored liquid, was chloride-free and satisfied the type A and type F requirements of ASTM Standard C494-2005 [29]. Potable water was used for both curing and casting. Mixing was performed using a Hobart mixer in accordance with ASTM Standard C 305-06 [30].
Compositions of the studied mortar mixtures
| Mix No. | Type of binder (%) | Amount of ingredient (kg/m3) | SP (%) | W/B ratio | S/B | |||||
|---|---|---|---|---|---|---|---|---|---|---|
| OPC | NC | GD | Binder | Fine aggregate | ||||||
| OPC | NC | GD | ||||||||
| CM | 100 | 0 | − | 692 | − | − | 1,557 | 1.2 | 0.38 | 2.25 |
| 1.5NC | 98.5 | 1.5 | 0 | 681.6 | 10.4 | 0 | 1,557 | 1.2 | 0.38 | 2.25 |
| 3.0NC | 97.0 | 3.0 | 0 | 671.2 | 20.8 | 0 | 1,557 | 1.2 | 0.38 | 2.25 |
| 4.5NC | 95.5 | 4.5 | 0 | 660.9 | 31.1 | 0 | 1,557 | 1.2 | 0.38 | 2.25 |
| 10GD | 90 | 0 | 10 | 622.8 | 0 | 69.2 | 1,557 | 1.2 | 0.38 | 2.25 |
| 20GD | 80 | 0 | 20 | 553.6 | 0 | 138.4 | 1,557 | 1.2 | 0.38 | 2.25 |
| 30GD | 70 | 0 | 30 | 484.4 | 0 | 207.6 | 1,557 | 1.2 | 0.38 | 2.25 |
| 3NC10GD | 87 | 3.0 | 10 | 602 | 20.8 | 69.2 | 1,557 | 1.2 | 0.38 | 2.25 |
| 3NC20GD | 77 | 3.0 | 20 | 532.8 | 20.8 | 138.4 | 1,557 | 1.2 | 0.38 | 2.25 |
| 3NC30GD | 67 | 3.0 | 30 | 463.6 | 20.8 | 207.6 | 1,557 | 1.2 | 0.38 | 2.25 |
After mixing, a flow table test was performed to evaluate the fresh properties of the mortar mixes in accordance with ASTM Standard C1437 [31]. The properties of the hardened materials were then evaluated by measuring their bulk unit weight, compressive strength, and flexural tensile strength. Compressive strength was determined using molded mortar cubes (50 mm × 50 mm × 50 mm), while flexural strength was determined using molded mortar prisms (100 mm × 100 mm × 500 mm). The molds were cleaned and polished internally with oil to avoid adhesion. The CMs were placed in molds in two layers, and air bubbles were removed from each layer using a vibrating table for 1 min each. After casting, the specimens were covered with plastic sheets for 24 h to prevent water evaporation and plastic shrinkage cracking. After 1 day, the molds were opened and the mortar specimens were immersed in a clean water bath at a temperature of 25°C ± 2°C until the testing age was reached. Bulk density was measured by crushing cube specimens after 7 and 28 days of aging as the weight per unit volume of mortar according to ASTM Standard C642-03 [32]. Compressive strength was measured using cube samples aged for 7, 28, and 90 days in accordance with ASTM Standard C 109-03 [33]; the reported values are the averages for three cubes. The compressive strength was determined using a control compression machine (made in Italy, tested in Iraq), with a loading speed of 0.24 MPa/s.
Flexural strength tests were performed using the two-point loading test with mortar prism samples after 28 days of aging, in accordance with ASTM Standard C348-02 [34]. The reported flexural strengths are the mean values for two beams.
3 Results and discussion
SAI values for the mortar cubes at 7 and 28 days are presented in Table 2. The pozzolanic activity of samples containing GD was 38% lower than that of control CM samples after 7 days’ aging and 21% lower after 28 days’ aging; in both cases, the values were very close to the minimum value specified in ASTM Standard C618 [35].
Flow test results for the mixes containing OPC, OPC + NC, OPC + GD, and OPC + NC + GD are shown in Figure 3. Increasing the replacement percentage of cement with NC, GD, or NC + GD from 0% (control CM) to 33% (for the 3NC30GD blend) reduced the flowability of the mortars, resulting in increasingly sticky mixes. This is presumably because NC and GD are fine materials with a high SSA, so their presence increases the mixture’s water demand and alters its consistency due to the higher water absorption [36,37], and other studies have shown that it can be necessary to increase the water content of mortar to achieve a desired consistency in cases where the addition of pozzolanic materials reduces flowability [22,38,39]. The water demand required to workability depends on the amount of free water filling the interparticle space and the amount of water adsorbed onto inner and outer pore walls.
Flow test results for the studied mortar mixes.
Figure 4 shows the effects of replacing cement with NC, GD, or GD + NC on the bulk density of specimens cured in water for 7 and 28 days. For all mixes, the bulk density increased with age. As shown in Tables 2 and 3, the specific gravities of the NC and GD used in this work were lower than that of the OPC. The bulk densities of the samples therefore decreased as the amount of OPC replaced by NC and GD increased in both binary and ternary blends binders, and the 3NC30GD mix yielded the lowest bulk density.
Bulk densities of the studied mortar mixes at 28 days.
The compressive strength measurements (Figures 5 and 6) showed that compressive strength of cubes made using all of the studied mixes increased steadily over time. Substituting OPC with NC and GD significantly affected the compressive strength at all ages. Increasing the content of NC in the mixes increased compressive strength to the control CM mix until the NC replacement percentage reached 3.0% by weight; further increasing the NC content reduced the compressive strength. The increased compressive strength could be due to the pozzolanic reaction of NC, its high SSA, and the greater fineness of the NC particles when compared to cement, which would be expected to result in a faster pozzolanic reaction and the formation of a denser structure matrix [40].
Compressive strengths of mortar mixes containing NC and GD at different ages.
Compressive strengths of mortar mixes containing NC + GD at different ages.
After 7 days of aging, the compressive strength for all mortar mixes containing GD or NC + GD was slightly lower than that for the control mix. Conversely, after 28 and 90 days of aging, the compressive strengths of these mixes were higher than those for the control mix. Mix 3CN10GD, which contained 3% NC and 10% GD, yielded the highest compressive strength in samples aged for 28 or 90 days, as shown in Figure 6. This improvement in strength is probably due to several factors, including the contribution of NC as filler due to the high SSA and the fineness of NC particles, and the rapid pozzolanic reaction of NC with Ca(OH)2, which would be expected to increase early strength when compared to mixtures containing only GD. Subsequently, NC acts as pozzolanic material by participation in the hydration process of cement [41].
The combination of NC and GD resulted in the greatest enhancement of strength at later ages. The mixture in which NC and GD replaced 3 and 10% of the OPC binder, respectively, offered the highest compressive strength while not excessively reducing workability.
When the GD replacement percentage was increased to 20 or 30% in mixes 20GD and 30GD, the compressive strength was slightly lower than that of the CM. This could be because of the slower hydration reaction of GD, which is presumably also why GD mixes had lower compressive strengths at 7 days than mixes containing only NC. Similar results were reported previously [20,22]. Ternary mixes containing both NC and GD had higher compressive strengths than mixes containing GD alone, probably due to the greater pozzolanic reactivity and fineness of the NC particles when compared to GD particles. Furthermore, the increase in compressive strength of CM containing NC is due to amorphous state of NC (small particle size) and extremely large surface area, in which the NC reacts more quickly with free lime in the hydration reaction than NC and subsequently produced more secondary C–S–H gel and filled the capillary pores in the matrix efficiently [41,42]. Despite this, as shown in Tables 1 and 2, the GD had a higher SSA, higher contents of silica and alumina, and a lower LOI than OPC, making it a suitable alternative binder like other established supplementary cementitious materials.
The tensile-to-compressive strength ratio of a mortar or concrete depends heavily on its compressive strength. The flexural strengths of the studied mortar mixes after 28 days of curing are shown in Figure 7. As can be seen, the trends in flexural strength mirrored those for compressive strength (Figures 5 and 6): flexural strength increased with the content of NC until the NC content reached 3%, and the flexural strength for mixes containing 3% NC was up to 18.5% higher than that for the control CM mortar. The flexural strength of the 10GD mix was also higher than that of the control CM, in accordance with the findings of Sounthararajan and Sivakumar (2013) [43]. The mix containing 3% NC and 10% GD thus maximizes both flexural and compressive strength at 28 days. This is likely due to the fineness of the NC and GD and their pozzolanic effect, as discussed earlier.
Flexural strengths of all mortar mixes at 28 days.
The results for the ternary CMs (OPC + NC + GD) show that the addition of 3% NC significantly increased flexural strength after 28 days of aging when compared to the corresponding mixes containing only GD (10GD, 20GD, and 30GD). The flexural strength of the optimal 3NC10GD mix after 28 days was 13.1% higher than that of the control CM mix. These results show that using NC as a binder to partially replace cement significantly improved strength after 28 days of aging.
4 Conclusions
The physical properties of CM mixes containing OPC, NC, and GD as binders have been investigated experimentally, yielding the following conclusions:
Partial replacement of OPC with NC and GD increased the water demand of the mortar mixes. Increasing the proportion of OPC replaced with NC and/or GD reduced workability and flowability relative to the control (OPC only) mix because of the greater fineness of the NC and GD particles.
The bulk density of the mortar increased as the substitution of OPC with NC and GD increased. The lowest bulk density was seen for the 3NC30GD mix with 3% NC and 30% GD substitution.
The compressive strength of the mortar mixes increased with the NC content at all test ages. An NC replacement proportion of 3% by weight of cement was found to be superior to 1.5 or 4.5% NC substitution in terms of compressive strength. All mortar mixes containing GD exhibited a slight reduction in early-age (7 days) compressive strength relative to the control CM but had higher compressive strengths after 28 and 90 days of aging.
The 3NC10GD mix, in which 3% of the OPC was replaced with NC and 10% was replaced with GD, had the highest compressive and flexural strengths of all the tested mixes, including the control mortar. Conversely, mixes with 20 and 30% GD replacement had slightly lower strengths than the control mortar.
Flexural strength increased with the content of NC; the flexural strength of the mix with 3% NC replacement was 18.5% higher than that for the control mortar. The optimal GD replacement proportion in terms of flexural strength was 10%. Adding 3% NC to mixes containing 10, 20, or 30% GD increased their flexural strength; the flexural strength of the 3NC10GD mix was 13.1% higher than that of the control mix. The optimal 3NC10GD mix had higher compressive and flexural strengths than the control mortar at all ages. Conversely, mixes with 20 or 30% GD replacement had slightly less strength than the control mortar mix.
5 Future prospective
In laboratory work, several mix designs of CMs have been developed by using GD and NC as a partial replacement of cement in binary and ternary blended in construction materials is recommended because it contributes to the enhancement of CM properties. In future studies, the durability assessment of CMs containing NC and GD should be conducted to understand the reaction of NC and GS under the severe attack environment and the effect of long-time use of these materials on the properties of cement blended in binary and ternary mortar mixtures.
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Funding information: The authors state no funding involved.
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Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.
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Conflict of interest: The authors state no conflict of interest.
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