From Nanostructural Characterization of Nanoparticles to Performance Assessment of Low Clinker Fiber–Cement Nanohybrids
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials and Nanomaterials
- Portland limestone cement CEMII/A-L42.5, with a limestone content of 14%, conforming to EN 197-1. The supplier gave the following clinker composition: 70% C3S, 4% C2S, 9% C3A, 12% C4AF. CEM II/A-L42.5. In mix proportioning the Portland cement (PC) content (86% by mass) was considered separately from the limestone (LS) content (14% by mass)
- Limestone (additional LS), conforming to EN 197-1. The total LS content of each paste was the sum of that contained in the Portland limestone cement and this additional LS.
- Fly ash (FA), conforming to EN 450. The oxide composition provided by the material data sheet was: 53.5% SiO2, 34.3% Al2O3, 3,6% Fe2O3, 4.4% CaO.
- Organomodified nano-montmorillonite (nMt), nC2 dispersed in water with the help of an alkyl aryl sulfonate surfactant, containing about 15% by mass of nMt particles.
- Inorganic nano-montmorillonite (nMt), nC3 dispersed in water with the help of sodium tripolyphosphate, containing about 15% by mass of nMt particles.
- Organomodified nano-montmorillonite (nMt), nC4, an industrial product by Sigma-Aldrich, non-dispersed—in powder form. It consists of Montmorillonite K-10 (70–75 wt%) surface modified with 25–30 wt% methyl dihydroxyethyl hydrogenated tallow ammonium * Nanomer® I.34 MN. The supplier’s data sheet gives the following additional information: 6.5 < pH < 7.0 and density = 1.7 g/cm3.
- PVA fibers, kuralon H-1, 4 mm, added at 2% by weight.
- Superplasticizer viscocrete 20 HE, denoted as SP.
2.2. Methods
2.2.1. Formulation of Fiber–Cement Nanohybrids
- Dry mixing of all powder components was firstly carried out with a spatula by hand. For the powder nMt, mixing was carried out together with PC and LS.
- For formulations containing nMt in dispersion, the nC2 or nC3 dispersion was poured in a separate container together with water, stirred with the use of a magnetic stir bar for 1 min, and then added to the mixed powders.
- The PVA fibers were added last after they had been manually further separated.
- With the addition of water (and nC2/nC3 where applicable), the paste was mixed employing a dual shaft mixer at 1150 rpm for a duration of up to four min.
2.2.2. Analytical Testing
3. Results and Discussion
3.1. Characterization of nMt Powder (nC4)
- nC2 compared to nC4 has higher potential to form additional C–S–H, due to the higher quantities of silica and limited exfoliation. At the same time, the greater amount of carbon present is expected to cause reduction in compressive strengths [19].
- The inorganic nMt, nC3, exhibited the highest net amounts of Si and Al, essential for C–S–H and C–Al–H.
- Traces of Na were found in the nC2 dispersion, because an anionic surfactant containing Na was used.
- The pronounced presence of Na in nC3 proves that nC3 was formed by a natural sodium-MMT, whereas the absence of Na in sample nC4 implies that nC4 was not a sodium-MMT originally.
- The Ca content in nC3 could potentially take part in the C–S–H forming hydration reactions or acting as a seeding agent [13].
- Compared to nC2, the commercially available nC4 was better exfoliated, but showed marginally greater variation in Si/Al and more polycrystalline phases.
- Up to 200 °C, the mass loss is associated with adsorbed interlayer water. Therefore, in the case of the inorganic MMT, a significant mass loss is observed.
- Between 200 and 500 °C the mass loss is associated with the decomposition of organic elements (modifiers and surfactants) attached to the MMT platelets usually exhibiting two peaks due to different structural arrangements. This is the area in which the main differences between the OMMT’s are identified and, hence, the powder OMMT and the dispersed OMMT of this study are distinctively different, even though similar organic salts were used for the separation of the platelets.
- Between 550 and 800 °C, the mass loss is associated with the loss of structural water from the MMT, known as dihydroxylation. Again, this is the area in which mass changes are expected and observed for the inorganic MMT.
- In the temperature range of 30–130 °C, with a distinct peak at 67 °C, attributed to the loss of surface and interlayer water.
- In the temperature range of 200–330 °C, with a distinct peak at 295 °C, the decomposition of modifier bound to neighboring molecules took place.
- In the temperature range of 330–530 °C, with a distinct peak at 396 °C, the deconstruction of the modifier bound to the bentonite was completed.
- In the temperature range of 570–700 °C, with a distinct peak at 600 °C, the remaining OMMT was decomposed.
3.2. Characterization of Fiber–Cement Nanohybrids
3.2.1. Flexural Strength
3.2.2. Thermal Gravimetric Analyses
3.2.3. Crystallographic Analyses (XRD)
3.2.4. Relative Density, Water Impermeability Analyses, and Mercury Intrusion Porosimetry (MIP)
3.2.5. Water Impermeability Tests
3.2.6. Mercury Intrusion Porosimetry (MIP)
4. Conclusions
- Extends from the characterization of nanoparticles to the characterization of fiber–cement nanohybrids.
- Is applied to ternary fiber–cement nanohybrids directly.
- Compares the effect of hydrophilic or hydrophobic nMt.
- Compares the effect of dispersed hydrophobic nMt or powder hydrophobic nMt.
- Correlates the flexural performance beyond day 28, an indeed more critical period, with the TGA results relating to the consumption of Ca(OH)2 towards the production of C–S–H.
- The organomodified aqueous dispersion of nMt, nC2, can be better developed as a material by studying various combinations of production methods, such as ball milling, in order for the product to necessitate lower amounts of modifier (i.e., less carbon addition).
- The inorganic aqueous dispersion of nMt, nC3, offered strength, thermal, and microstructural improvements.
- The industrial powder nMt, nC4, did not offer any strength, chemical, or microstructural enhancements.
- Different methods for nMt dispersion in cementitious matrices can be assessed in future research to achieve homogeneous mixing and easy compaction, which should reflect in the pore structure and fresh properties of pastes.
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Manufacturing and Fabrication Method | Cement Mix | Characterization Technique | Selected Results | Reference |
---|---|---|---|---|
Ultrasonic sonication | Ordinary Portland cement (OPC) type 42.5R and commercially available nano-kaolinite clay (NKC) powder was added as Portland cement (PC) replacement at 0%, 1%, 3%, and 5% by weight. The NKC was first dispersed in water using an ultrasonic dispersion method. | X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM) techniques were carried out on the clay powder. | The samples with 5% NKC exhibited the highest compressive strength, chloride diffusion resistivity, relative dynamic modulus of elasticity, and the most electrical resistivity after 125 freeze–thaw cycles. | [23] |
Hobart electric mixer | OPC is partially substituted by 1%, 2%, or 3% nanoclay by weight of OPC. The OPC and nanoclay were first dry mixed for 5 min in Hobart mixer at a low speed and then mixed for another 10 min at high speed until homogeneity was achieved. Cloisite30B is a natural montmorillonite modified with a quaternary ammonium salt, which was supplied by Southern Clay Products, USA. | X-ray diffraction (XRD) analysis. | The nanoclay behaves not only as a filler to improve microstructure, but also as an activator to promote pozzolanic reaction. | [24] |
Electric mixer | OPC mortars where produced by partial substitution with NMK at 2%, 4%, 6%, and 8% by weight of cement. The nanoclay used in this investigation is kaolin clay supplied by Middle East Mining Investments Company (MEMCO), Cairo, Egypt. The nano-kaolin was heated for 2 h at 750 °C to give active amorphous NMK. The ingredients were homogenized on an electric mixer to assure complete homogeneity. | TEM imaging of NMK. | The compressive strength and the tensile strength of the cement mortars with NMK were higher than the reference mortar at the same water to binder (w/b) ratio. The enhancement in tensile strength reached 49%, whereas the enhancement in compressive was 7% at 8% NMK. | [25] |
Electric mixer | A total of 1% or 2% Nano-montmorillonite modified foamed paste was produced with a high volume (70%) fly ash binder. The nMt used was produced by Zhejiang FengHong New Materials Co., Ltd., which has a purity of 99.5% (Technical Grade) The foaming agents and stabilizing agent had been dissolved in the water and used to soak the nMt for 24 h to facilitate its dispersion. Solids were mixed first and then mixed with water. Lastly, with the water containing nMt and foaming agents. | Not applicable. | Mix constituting of 70% FA, 1% alpha-olen sulfonate (AOS), 2% alcohol ethoxylate (AEO), 0.75% Na3PO4 and 1% nMt) exhibited the lowest thermal conductivity (0.071 W (m1 K1)) and reasonably high strength (3.23 MPa) at 28 days. | [22] |
Electric mixer and ball mill | The blended cement paste samples were prepared by partial replacement of cement with 2%, 4%, 6%, 8%, 10%, 12%, and 14% nano-metakaolin (NMK) by weight of cement. All pastes were prepared with the same water to cement (W/C) ratio 0.3. The ingredients of the blended cement pastes were homogenized on an electric mixer to assure complete homogeneity. The NMK was thermally treated at 750 °C for 2 h to assure complete decomposition and to get active amorphous nano-metakaolin (NMK). The ingredients were homogenized on a roller in a porcelain ball mill with four balls for 1 h to assure complete homogeneity. | Differential thermal analysis (DTA) was performed for the nano-kaolin to specify the decomposition/calcinations temperature. XRD to confirm that the kaolinite phase transformed into amorphous phase TEM imaging confirmed the thermal activation, capturing reduction in grain size with ill-defined edges, which suggests some amorphous character and results in increasing the pozzolanic reactivity of NMK. | The optimum replacement was found to be 10% with which an enhancement of compressive strength by about 50% and flexure strength by 36% was achieved. Microstructure was also enhanced. | [26] |
Distilled water and stirring for the OMMT, then electric mixing of the cementitious nanocomposites | Ordinary Portland cement type CEM II/A-LL 42.5 N (OPC) and OMMT at 1% cement replacement and at water to solid ratio (w/s) equal to 0.27. Sodium MMT (cation exchange capacity (CEC) 105 meq/100 g), was used for OMMT synthesis in the laboratory by applying the ion exchange method. Quaternary ammonium salt (QAS) methylbenzyl di-hydrogenated tallow ammonium chloride (Noramium MB2HT = 640 g/mol) was selected as a modifier to produce three OMT denoted as 06, 08, and 1 M, respectively (corresponding to 0.6, 0.8 and 1.0 cation exchange degree). Each OMMT was mixed with distilled water and stirred rigorously for one day at 20 °C, to ensure the formation of well-dispersed suspension. After stirring time terminated, the OMMT–water suspension was mixed with the required amount of cement. | The pozzolanic activity of the modified clays was determined by the Frattini test. | The properties of OMMT modified cement paste vary according to the cation exchange degree of the OMMT. OMMT of lower cation exchange degree (0.6 M) shows pozzolanic behaviour after 14 days, while OMMT of higher cation exchange degree (0.8 and 1 M) displays the activity later only after 28 days. | [27] |
Sample | PC (%) | LS (%) | nMt (%solids) | SP (%) | PVA fibres (%) | W/S |
---|---|---|---|---|---|---|
F.PC60LS40PVA3SP2+0%nC | 60 | 40 | 0 | 2 | 3 | 0.3 |
F.PC60LS39PVA3SP2+1%nC2 | 60 | 39 | 1 | 2 | 3 | 0.3 |
F.PC60LS39PVA3SP2+1%nC3 | 60 | 39 | 1 | 2 | 3 | 0.3 |
F.PC60LS39PVA3SP2+1%nC4 | 60 | 39 | 1 | 2 | 3 | 0.3 |
Initially Undispersed nC—All Results in Atomic % Normalized by 100% | ||||||
---|---|---|---|---|---|---|
Spectrum | C | O | Mg | Al | Si | Fe |
(1, 1) | 38.63 | 49.13 | 0.55 | 3.29 | 8.01 | 0.40 |
(2, 1) | 39.31 | 45.63 | 0.62 | 3.94 | 9.95 | 0.54 |
(3, 1) | 37.94 | 48.55 | 0.60 | 3.70 | 8.74 | 0.47 |
(4, 1) | 39.87 | 48.95 | 0.47 | 2.86 | 7.40 | 0.44 |
(5, 1) | 38.78 | 47.83 | 0.55 | 3.54 | 8.83 | 0.47 |
Total mean | 41.01 | 45.56 | 0.51 | 3.37 | 8.30 | 1.25 |
Standard Deviation | 2.95 | 2.95 | 0.08 | 0.52 | 1.47 | 0.99 |
0–100 °C | 100–250 °C | 250–400 °C | 400–500 °C | 500–700 °C | |
---|---|---|---|---|---|
nC4 | 1.33 | 0.31 | 13.63 | 8.00 | 2.86 |
Mercury Intrusion Data Summary at 28 Days | ||||||||
---|---|---|---|---|---|---|---|---|
Paste | Apore-Total (m²/g) | Fpore Volume-Med (nm) | Fpore Area-Med (nm) | Rbulk (g/mL) | Fpore-Average (nm) | Rapparent (g/mL) | Porosity (%) | Vstem-Used (%) |
F.PC60LS40PVA3SP2 | 45.8 | 76.8 | 5.1 | 1.6 | 18.9 | 2.4 | 34.1 | 50.0 |
F.PC60LS39PVA3SP2+1%nC3 | 51.2 | 29.1 | 5.5 | 1.7 | 14.1 | 2.5 | 30.6 | 37.0 |
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Papatzani, S.; Paine, K. From Nanostructural Characterization of Nanoparticles to Performance Assessment of Low Clinker Fiber–Cement Nanohybrids. Appl. Sci. 2019, 9, 1938. https://0-doi-org.brum.beds.ac.uk/10.3390/app9091938
Papatzani S, Paine K. From Nanostructural Characterization of Nanoparticles to Performance Assessment of Low Clinker Fiber–Cement Nanohybrids. Applied Sciences. 2019; 9(9):1938. https://0-doi-org.brum.beds.ac.uk/10.3390/app9091938
Chicago/Turabian StylePapatzani, Styliani, and Kevin Paine. 2019. "From Nanostructural Characterization of Nanoparticles to Performance Assessment of Low Clinker Fiber–Cement Nanohybrids" Applied Sciences 9, no. 9: 1938. https://0-doi-org.brum.beds.ac.uk/10.3390/app9091938