Applications of Nanotechnology in Cement and Concrete Science

Handbook of Research on Diverse Applications of Nanotechnology in Biomedicine, Chemistry, and Engineering

Shivani SoniAlabama State University, USA

Amandeep SalhotraCity of Hope National Medical Center, USA

Mrutyunjay SuarKIIT University, India

A volume in the Advances in Chemical and Materials Engineering (ACME) Book Series

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Handbook of research on diverse applications of nanotechnology in biomedicine, chemistry, and engineering / Shivani Soni, Amandeep Salhotra, and Mrutyunjay Suar, editors. pages cm Includes bibliographical references and index. ISBN 978-1-4666-6363-3 (hardcover) -- ISBN 978-1-4666-6364-0 (ebook) -- ISBN 978-1-4666-6366-4 (print & perpetual access) 1. Nanotechnology. I. Soni, Shivani, 1975- II. Salhotra, Amandeep, 1975- III. Suar, Mrutyunjay, 1975- T174.7.H375 2014 620’.5--dc23 2014022017

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Chapter 29

Applications of Nanotechnology in Cement and Concrete Science

ABSTRACT

The properties of concrete are strongly influenced by the properties of its components and hydrates at the nanoscale. Therefore, application of nanotechnology in cement and concrete science will engender new opportunities for improvement of strength and durability of concrete. The objective of this chapter is to advance the science and engineering of nanotechnology in modifying and monitoring the behaviour and performance of cement and concrete at the nanoscale. The chapter assists in the identification of promising new research and innovations in concrete materials using nanotechnology that can result in improved mechanical properties, volume change properties, durability, and sustainability. The chapter also provides a unique base for scientists, engineers, and practitioners to help set the future direction of the use of nanotechnology in cement and concrete science.

INTRODUCTION

Nanotechnology is an appearing field of research associated to the understanding and command of issue at the nano scale, i.e., at dimensions between approximately 1 and 100 nm. At the nano scale, unique phenomena endow novel submissions. Nanotechnology encompasses nano scale science, technology, and expertise that engage imaging, measuring, modelling, and manipulating issue at this extent scale. Nano scale particles are not new in either environment or research. Latest develop-ments in visualization and estimation systems for

characterizing and checking components at the nano scale have led to a blast in nanotechnology-based components in areas such as polymers, plastics, electronics, vehicle constructing and surgery (Duncan, 2011). Issue can display unusual physical, chemical, and biological properties at the nano scale, differing in significant ways from the properties of bulk components and single atoms or substances. Some nanostructured components are more powerful or have distinct magnetic properties contrasted to other forms or sizes of the identical material. Others are better at carrying out heat or electricity (Ma et al., 2008). They may become

Salim BarbhuiyaCurtin University of Technology, Australia

Muneeb QureshiCurtin University of Technology, Australia

DOI: 10.4018/978-1-4666-6363-3.ch029

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more chemically reactive or contemplate light better or change colour as their dimensions or structure is changed (Baddeley et al., 2007).

Working at the nano scale endows scientists to utilize the unique personal, chemical, mechanical, and optical properties of components that routinely occur at that scale. Specific relevance for solid is the greatly advanced surface locality of particles at the nano scale. As the surface area per mass of a material rises, a greater amount of the mate-rial can arrive to communicate with surrounding materials, therefore affecting reactivity. Nanotech-nology considers two major advances as shown in Figure 1: the ‘‘top down” approach in which bigger organisations are decreased in dimensions to the nano scale while sustaining their original properties without atomic-level control (e.g., miniaturization in the domain of electronics) or deconstructed from bigger organisations into their lesser composite components and the ‘‘bottom-up” approach, furthermore called ‘‘molecular

nanotechnology” or ‘‘molecular constructing” in which components are engineered from atoms or molecular components through a method of assembly or self-assembly.

The mechanical properties of cement and concrete depend to a large extent on structural elements and phenomena, which are effective on a micro- and nanoscale (Shah et al., 2011). Nanotechnology has the potential to engineer concrete with superior properties through the optimization of material behavior and performance needed to significantly improve mechanical per-formance, durability and sustainability. The use of nanotechnology is likely to make various key breakthroughs in cement and concrete technology. Better understanding and precise engineering of an extremely complex structure of cement-based materials at the nano-level will result in a new generation of concrete, stronger and more durable, with desired stress-strain behavior and possibly possessing the range of newly introduced “smart”

Figure 1. Top down and bottom up approaches in nanotechnology

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properties. The advances in instrumentation and computational science are enabling scientists and engineers to obtain unprecedented information about concrete, from the atomic through the con-tinuum scale, and the role of nanoscale structures on performance and durability. This information is crucial for predicting the service life of concrete and for providing new insights on how it can be improved (Sanchez & Sobolev, 2010).

Better understanding and mimicking the pro-cesses of “bottom-up” construction successfully employed by nature is one of the most promising directions in nanotechnology (Bhushan, 2004). It was proved that the exceptional mechanical performance of biomaterials, such as bones or mollusk shells, is due to advanced nanostructure and the reinforcing action of nanocrystals of calcium compound. High tensile strength macro-defect-free (MDF) cement is a polymer-cement composite, which mimics the structure of the abalone shells at the micrometer and nanometre levels. Improved performance of MDF is attributed to the grafting of polymer chains onto the surface of cement grains.

NANO-MODIFICATION OF CONCRETE

From nanotechnology point of view, hardened cement itself is clearly a nanomaterial without any modification. This is because it has a hier-archical structure ranging from sub-millimetre dimension down to nanometre scale. The general view on length scale and surface areas related to concrete making materials and additives is shown in Figure 1. Moreover, it is also well established that most of its material properties mainly depend on the microstructural development below 100nm (Taylor, 1997).

In the last decades there has been a continu-ously increasing trend to modify and optimize cementitious binders by means of nanotechnology and nanoscale additives. Supramolecular additives in cement and concrete are known and used since

the mid-1960s. They can act as high performance dispersants, rheology modifier or anti shrinkage agents. They control rheological properties of the cement paste by electrostatic, hydrophobic or steric interactions. The development of improved supramolecular additives allowed incorporation to a certain extent, nanoscale filler particles and materials into cement paste and concrete mixes. These fillers are mostly inert and they neither interfere with the hydration process nor do they change the hydration products. Their main task is to optimize the grain size distribution leading to a highly filled and compact cement matrix with reduced pores and voids. The latest means of nano-modification of cementitious systems are functional nano additives, which influence hydration and/or structure development. Known systems comprise of nano-tubes or nano-rods (Akkaya et al., 2003; Trettin & Kowald, 2005; Shah et al., 2009), nanoscale C-S-H particles and nanoscale gypsum particles. They act as internal reinforcement as well as nucleation and crystal-lization seeds.

SUPERHYDROPHOBIC CONCRETE

The leaves of the lotus plant (Nelumbo Nucifera) naturally have superhydrophobic and self-cleaning surfaces. This provides an excellent example of how biomimetics can be used for an effective engineering design (Bhushan, 2004). The superhy-drophobicity of most plant surfaces is achieved by hierarchical structures of convex or papilla epider-mal cells with three-dimensional wax structures on top. The hierarchical (double-structured) surface is characteristic for the lotus leaf, which is built of convex cells and has a much smaller superimposed layer of hydrophobic, three-dimensional wax tubules. Wetting of such surfaces is minimized, because air is trapped in the cavities of the convex cell and the hierarchical roughness enlarges the water-air interface while reducing the solid-water interface. Water on such a surface gains very little energy through adsorption and forms a spherical

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droplet. Therefore, both the contact area and the adhesion to the surface are dramatically reduced. The superhydrophobic and self-cleaning surfaces of a flowering plant of lotus (Nelumbo Nucifera) is shown in Figure 3a; a lotus leaf contaminated with clay is shown in Figure 3b; removal of the adhering particles by water is shown in Fig 2c; a spherical water droplet on a superhydrophobic leaf is shown in Figure 3d; the SEM image of a droplet (Figure 3e) illustrates the low wettability of superhydrophobic microstructured surfaces; the SEM images 3f, 3g and 3h show the Lotus leaf surface in different magnifications (Koch et al., 2008).

In concrete, superhydrophobicity can substan-tially improve the performance of conventional hydrophobic materials (e.g., siloxane-based, such as polyethyl-/polymethyl- hydrosiloxane, PEHSO/PMHS) and control the wettability of solid materials (Sobolev & Batrakov, 2007). Super-hydrophobic surfaces with a water contact angle (θ) larger than 150° (Figure 4) have generated much interest due to their potential in industrial applications (mainly for self-cleaning), and this nature-inspired concept was recently realized for enhancing concrete durability. To manufacture su-perhydrophobic admixture the hydrogen contain-ing siloxane (e.g., PEHSO/PMHS) is combined with small quantities of super-fine, submicro- or

Figure 2. Particle size and specific surface area related to concrete making materials (Sobolev & Ferrada-Gutiérrez, 2005)

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nano-sized particles such as nano-silica, nano-clay additives or SiO2-rich reactive powders (Sobolev et al., 2011). The volume, size and distribution of the air voids within the hardened cement phase can be precisely tailored by preparing the water-based PEHSO emulsion with a certain droplet size. Submicro- or nano-sized particles provide the micro-roughness within the pore space, which plays an important role in forming superhydrophobic surfaces within the hardened cement and improves the self-healing potential of concrete. The surfaces of the voids are covered by the hydrophobic particles, providing the effect of superhydrophobic hybridization.

USE OF NANO PARTICLES AND NANO REINFORCEMENT IN CONCRETE

Nanoparticles are gaining widespread attention to be used in construction sector so as to exhibit enhanced performance of materials in terms of smart functions and sustainable features. Incor-poration of various nanoparticles into the cement matrix to improve various properties of concrete emerged as a promising research filed of nano-composites. In cement matrix, most of the research to date was conducted on nano-silica (nano-SiO2) (Bjornstrom et al. 2004; Li et al., 2004; Li et al.,

Figure 3. Superhydrophobic and self-cleaning surfaces of a flowering plant of lotus (Nelumbo Nucifera)

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2006; Sobolev et al., 2009; Qing et al., 2008) and nano-titanium oxide (nano-TiO2) (Li et al., 2006; Li et al., 2007). A few studies on the incorpora-tion of nano-iron (nano-Fe2O3) (Li et al., 2004), nano-alumina (nano-Al2O3) (Li et al., 2006) and nano-clay particles (Chang et al., 2007) in cement matrix are also reported. Research (Sobolev & Ferrada-Gutiérrez, 2005) showed that nano-SiO2 (Figure 5) improves the workability and strength of concrete.

The incorporation of nano-SiO2 in concrete was also found to increase the water penetration resistance of concrete (Ji, 2005). Gaitero et al., (2008) have demonstrated that use of nano-SiO2

can help to control the calcium leaching in con-crete. It is also reported that nano-SiO2 is more effective than microsilica in enhancing the strength properties of concrete (Jo et al., 2007; Qing et al., 2007). Particles of nano-SiO2 not only act as a filler material, but also they act as an activator to promote the pozzolanic reaction. Li (2004) reported that significant increase in compressive strength at early age could be obtained using nano-SiO2 in high volume fly ash concrete, which is one of the drawbacks of this type of concrete. However, in order to achieve good performance and to use nano-SiO2 in economical way, it is better to use nano- SiO2 in a combination of fly

Figure 4. Concept of super-hydrophobic hybridization of concrete pore surface (Sobolev & Sanchez, 2012)

Figure 5. Spherical nano-SiO2 particles of uniform distribution observed using TEM (Sobolev & Ferrada-Gutiérrez, 2005)

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ash and microsilica. According to Hosseini et al., (2010), nano-SiO2 improves the properties of the cement matrix by (i) providing a nucleation site, (ii) producing added amount of C-S-H gel through pozzolanic reaction, (iii) controlling crystalliza-tion and (iv) modifying the microfilling effect.

Nano-Al2O3 is very useful to modify the modu-lus of elasticity of cement mix. The addition of nano-Al2O3 was also found to be very effective to increase the elastic modulus of mortar. With the addition of 5% nano-Al2O3, Li et al., (2006) found that there was an increase of 143% in the elastic modulus. However, the authors reported that they had a limited effect on the compressive strength. Recent research by Barbhuiya et al., (2014) has shown that proper dispersion is one of the major problems in using nano-Al2O3. The SEM image (Figure 6) of hydrated cement paste containing 2% nano-Al2O3 clearly shows the agglomeration of nano-Al2O3. Nano-Fe2O3 is reported to provide

concrete the self-sensing capacity (Li et al., 2004). Their inclusion also improves the compressive and flexural strength of concrete.

The sensing capabilities of concrete are in-valuable not only for real time structural health monitoring, but also for the construction of smart structures. This is simply because they do not invoke the use of embedded or attached sensors. Kawashima et al., (2013) observed that nano nano–CaCO3 take part in accelerating heat of hydration, setting time and upgrading compres-sive strength of concrete. Sonication improved the implications of nano-CaCO3 in each scenario. Nano-TiO2 has been identified as a potential nanomaterial with wide range applications. This is mainly because of its strong oxidizing capacity under U-V radiation, chemical stability, chemical inertness in absence of U-V light and absence of toxicity. The photocatalytic Nano-TiO2 is ener-gized by UV and accelerates the decomposition

Figure 6. SEM image of cement paste of containing 2% nano-Al2O3 hydrated for 7 days (Barbhuiya et al., 2014)

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of organic particulates and airborne pollutants such as nitrous oxide (NOx) as shown in Figure 7. Studies (Jayapalam et al., 2009) have shown that nano-TiO2 can accelerate early age hydra-tion of Portland cement. They are also found to improve the compressive and flexural strengths of concrete (Li et al., 2007). The authors also found that the abrasion resistance of concrete containing Nano-TiO2 is better than that containing the same amount of nano-SiO2. Nano-TiO2 has proven to be very effective to produce “self-cleaning” and “depolluting” concrete (Murata et al., 1999; Val-lee et al., 2004). Nano-TiO2 based “self-cleaning” concrete products are commercially available.

Carbon nanotubes/nanofibres (CNTs/CNFs) are potential candidates for use as nano rein-forcements in concrete. CNTs/CNFs exhibit extraordinary strength with moduli of elasticity on the order of TPa and tensile strength in the range of GPa, and they have unique electronic and chemical properties (Srivastava et al., 2003).

CNTs/CNFs, thus, appear to be among the most promising nanomaterials for enhancing the me-chanical properties of concrete and their resistance to crack propagation while providing such novel properties as electromagnetic field shielding and self-sensing (Makar et al., 2005; Li et al., 2007).

Single-wall CNTs (SWCNTs), multi-wall CNTs (MWCNTs), and CNFs are highly struc-tured graphene ring-based materials with very large aspect ratios (of 1000 or more) and very high surface areas. SWCNTs are single graphene cylinders and MWCNTs are multiple, concentric graphene cylinders coaxially arranged around a hollow core. Unlike CNTs, CNFs present nu-merous exposed edge planes along the surface that constitute potential sites for advantageous chemical or physical interaction. While CNTs/CNFs have been extensively studied in polymeric composites (Hammel et al., 2004; Coleman et al., 2006; Lau et al., 2006) their use in cement has, to date, remained limited. One of the main challenges

Figure 7. Photocatalytic nano-TiO2 is energized by UV

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is the proper dispersion of CNTs/CNFs into ce-ment paste, partly due to their high hydrophobic-ity and partly due to their strong self-attraction. Incorporating the unique mechanical properties of CNTs/CNFs in cement composites has proven to be rather complex and to date mixed results have been obtained. A number of methods have been investigated to improve dispersion and to activate the graphite surface in order to enhance the inter-facial interaction through surface functionalization and coating, optimal physical blending, and/or the use of surfactant and other admixtures.

NANOSCIENCE MODELLING OF CONCRETE

The hydration of Portland cement results in the formation of various products. Calcium Silicate Hydrate (C-S-H) is the dominant phase among the hydration products. It is produced during the reaction between the silicate phases (i.e. C3S and β-C2S) and water and forms up to 60% of the hydrated cement paste. C-S-H primarily contrib-utes to the important properties of the hardened concrete such as strength and volume stability. The nanostructure of this hydrated phase has not been fully resolved, and the debate over its structural properties still continues. Resolving the structure of this material at the nanoscale is an essential part of understanding and predicting its behaviour. The C-S-H gel is a nearly amorphous material that does not have a long-range ordered structure. The C-S-H gel is structurally related to the more ordered synthetic materials such as tobermorite and jennite. In these systems, layers of CaO are flanked on both sides by chains of silicate tetrahedra. A stacking of these sheets with water molecules, hydroxyl groups and calcium ions in between forms a C-S-H particle. Figure 8 shows a schematic of the tobermorite-like layer. The circles in the figure are calcium atoms located at the cen-tre of Ca-O octahedra (not shown); triangles are silicates- light gray: paired tetrahedra, dark gray:

bridging tetrahedra; hydroxyl groups, calcium ions and water molecules that may exist between the C-S-H sheets are not shown. The broad range of stoichiometries in C-S-H can be obtained by omitting the bridging tetrahedra, further defects in the silicate structure and inclusion of more calcium ions in the interlayer region (Cong & Kirkpatrick, 1996; Nonat, 2004; Chen et al., 2004).

The nanostructure of C-S-H is not fully re-solved although it has been the subject of much research. Several models have been suggested ranging from “gel-like” to “layer-like” to describe the physical properties of C-S-H. One of the first physical models was proposed by Powers and Brownyard, in which C-S-H was depicted as a gel-like material (Powers & Brownyard, 1947). In this model the gel particles are held together mainly by van der Waals’ forces and the space between them is called “gel porosity” that is accessible only by water molecules. A more comprehensive model was developed later by Feldman and Sereda (1968) based on extensive experimental studies of hydrated cement systems (Feldman & Sereda, 1968; Jennings 2008). The role of water in this model is explained in more detail. A schematic physical model for C-S-H in the hydrated Portland cement is shown in Figure 9, where the dark lines indicates tobermorite-like sheets, circles the physically adsorbed water and crosses the interlayer water. The main feature of the model is concerned with the layered nature of the C-S-H. Structural roles assigned to the in-terlayer water that exhibit irreversible behaviour during the adsorption and desorption processes. Changes in the mechanical properties of C-S-H related to water content can be easily described using this model.

Advancement in experimental techniques, has led to the development of new models. Jennings’ colloid model features globules of about 5nm in diameter for C-S-H and proposes the existence of intra-globular pores (IGP) and small gel pores (Jen-nings, 2008). The viability of using a layered model for the C-S-H in cement paste was more plausibly

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investigated using helium inflow technique as a nanostructural probe along with X-ray diffrac-tion method (Alizadeh et al., 2007). Changes at the nano-level in the properties of C-S-H(I), a layered semi-crystalline material, were followed upon the removal of adsorbed and interlayer water. The helium inflow results are analogous to those for C-S-H in hydrated Portland cement. They can be best explained by a layered model for C-S-H in cement paste.

Efforts have also been developed to model the behaviour of C-S-H at the nanoscale. Molecular dynamics have been used to model C-S-H (Gimra

et al., 2008). Molecular dynamic models based on free energy minimization techniques have been used to theoretically estimate the elastic proper-ties of C-S-H. It has been shown that the average Young’s modulus (E) increases with the increase in the C/S ratio of the C-S-H (Pellenq et al., 2007). The C/S ratio is not the only governing parameter in determining E and other factors such as the molecular arrangements and extent of water within the nanostructure of C-S-H may have an important role (Manzano et al., 2007). The bulk modulus of tobermorite was computed in two separate studies to be about 70 GPa (Gmira et al., 2007,

Figure 8. Simplified molecular structure of a single sheet of tobermorite-like material

Figure 9. A schematic physical model for C-S-H in the hydrated Portland cement

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Reinhardt et al., 2009). The discrepancy between the modelling simulations and the experimental results was attributed to the nano-structural de-fects in the silicate structure of tobermorite-like materials. Moreover, the finite element model was successfully used to model the nano-indentation response of cementitious materials.

NANOTECHNOLOGY-BASED DEVICES IN CONCRETE

Concrete durability can be improved with bet-ter quality control using wireless nanomachines known as Nano Electro Mechanical Systems (NEMS). Nanomachines are designed to measure durability affecting factors of concrete such as temperature, moisture, chloride, pH and carbon di-oxide along with density, viscosity during mixing and pumping, strength advancement and shrinkage stress in concrete (MaCoy et al., 2005). Whereas, properties such as internal relative humidity (RH) and temperature are measured with the help of microcantilever beams and moisture-sensitive thin polymer using Microelectromechanical systems abbreviated as (MEMS). Monitoring of temperature and moisture is necessary to evaluate the setting and hardening properties of concrete and foresee the possibility of occurrence of chemical distress in concrete e.g. corrosion of reinforcement, freeze-thaw distress, carbonation and alkali-aggregate reaction. MEMS has been observed to be an effective, durable and sensitive in measuring concrete temperature and moisture under internal/ external stresses and corrosive environment. However, some areas still needed further explorations such as long-term behaviour and repeatability of MEMS entrenched into con-crete, wireless interrogation e.g. signal orientation, data storage, processing, powering, communica-tion and computation capabilities.

CONCLUSION

Significant advancements have been made in the application of nanotechnology in cement and concrete science. There have been lots of improve-ments in understanding the characteristics of the hydration products of Portland cement (particu-larly C-S-H) at the nanoscale. This makes possible the development of better concrete that can address specific durability and environmental issues. The ability of nanoparticles to accelerate the rate of hydration of Portland cement opens the possibility of significantly lowering the content of cement in concrete. However, construction is unique, in that its products in the form of individual building and civil infrastructures are typically constructed from a vast combination of both conventional and new ‘high-tech” materials, using a relatively limited number of processes. Therefore, nanotechnology used in cement and concrete must be compatible to the traditional practices used in construction. Nonetheless, developing cement and concrete with the application of nanotechnology will have a sustained and important impact on the future of the construction industry.

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KEY TERMS AND DEFINITIONS

Microelectromechanical Systems: Micro-electromechanical Systems (MEMS) are tiny assimilated devices or systems that combine electrical and mechanical components. They range in size from the sub micrometre (or sub micron) level to the millimetre level, and there can be any number, from a few to millions, in single specific arrangement. MEMS extend the fabrica-tion methodologies established for the integrated circuit industry to add mechanical elements e.g. beams, gears, diaphragms, and springs to devices.

Molecular Nanotechnology: Molecular Nanotechnology abbreviated as MNT founded on the aptitude to build structures to complex, atomic specifications by means of mechanosynthesis.

Nano-Electromechanical Systems: Nano-electromechanical Systems (NEMS) are made of electromechanical devices possessing critical dimensions from hundreds to few nanometres.

Nano-Reinforcement: Nano reinforcement is a dispersion of nanoscale particles in the matrix during processing to enhance macroscale prop-

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erties of the composite materials. For example, addition of carbon nanotubes enhanced electrical and thermal conductivity of the material.

Nanotechnology: It is science, engineering, and technology conducted at nanoscale, about 1 to 100 nanometres (nano.gov). It includes study and applications of extremely small things and may be useful across all other science fields e.g. engineering, material science, physics, chemistry and biology.

Nucleation: Early-stage process that occurs in the formation of a crystal from a solution, a liquid, or a vapour, resulted in characteristic of

patterned arrangement of small number of ions, atoms or molecules forming a site on which ad-ditional particles are deposited as crystal grows is known as Nucleation.

Superhydrophobic Concrete: Superhydro-phobic Concrete is composite material prepared with cement-based materials with polyvinyl al-cohol fibers and superhydrophobic admixtures. It comprised of outstanding strength and durability. It has capability of replacing normal concrete in critical infrastructure components and provided with surprising lifespan of 120+ years.

Documents

Applications of Nanotechnology in Cement and Concrete Science