Novel Alkali-Activated Materials with Photocatalytic and Bactericidal Properties Based on Ceramic Tile Waste
2. Materials and Methods
2.2. Preparation of Alkali-Activated Materials
2.3. Characterization Techniques
- The average particle size of the CW precursor was determined using a Mastersizer 2000 laser granulometer (Malvern Instrument, Malvern, UK). The density of the CW raw material was determined by the pycnometer technique, following ASTM standard C127-04. The chemical composition of the CW and glass waste was determined with an Axios mAX sequential wavelength-dispersive X-ray fluorescence (WDXRF) spectrometer (PANalytical, Tollerton, UK) equipped with a rhodium tube and operated with a maximum power of 4.0 kW with SuperQ software version 5.0 L.
- The compressive strengths of the alkali activated materials were obtained according to ASTM C109 using 20 mm cubic specimens. The tests were carried out on an Instron 3369 universal testing machine (Instron, Norwood, MA, USA) at a displacement speed of 1 mm/min. The data reported correspond to the average of the four test specimens.
- The surfaces of the pieces obtained after the mechanical tests were observed with scanning electron microscopy (SEM) using a JEOL JSM-6490LV instrument (JEOL, Tokyo, Japan) with a 20 kV acceleration voltage. The pieces observed had been previously coated with gold, and the observations were made in high vacuum mode (3 × 10−6 torr). An Oxford Instruments Link-Isis X-ray spectrometer (Oxford Instruments, Abingdon, UK) was coupled to the microscope for energy-dispersive spectrometry (EDS).
- X-ray diffraction (XRD) of the CW and pastes was performed using an X’Pert MRD PANalytical (Malvern-PANalytical, Malvern, UK) diffractometer with Cu Kα1 radiation at 20 mA and 40 kV. The samples were scanned at 2θ angles between 5° and 60°, at a step rate of 0.02 and a holding time of 4.0 s per step.
- The physical properties of the pastes as the bulk density, percent absorption, and volume of permeable pores were determined according to ASTM C642, with the modification of leaving the samples submerged in water at 100 °C for 3 h instead of the 5 h specified in the standard for OPC-based materials. The data reported correspond to the average of the three test specimens.
- For the degradation of Rh-B, discs 3 cm in diameter and 4 mm in height were prepared from all pastes with 5 and 10 wt.% of TiO2 particles and ZnO particles. The determination of the photocatalytic activity was evaluated using a method based on that used by , performing the immersion of the samples in 10 mL of Rh-B with a concentration of 5 ppm, and using exposure to ultraviolet light for 24 h. UV-A radiation was supplied by two mercury lamps (ELECTROLUX T8 20w/BLB) located inside a black acrylic dome. These lamps emit light at an intensity of 10.3 W·m−2, which was measured with a Delta Ohm HD 2102.2 photoradiometer (Delta Ohm, Caselle, Italy) using the filter for UV-A light with a range of 5 mm. For each measurement, 1 mL aliquot was deposited in 50 mL of distilled water in a Falcon tube for centrifuge, and then a sample was taken and placed into quartz cell of 2 mL. The degradation efficiency after 24 h was monitored at a wavelength of 554 nm using a Shimadzu UV−VIS spectrophotometer (Shimadzu, Columbia, MD, USA), model UV-1800 series A1145450047OCD.
- The biological activity of the materials was evaluated through the inhibition of the bacterial growth  of ATCC strains of K. pneumoniae (ATCC® 13883TM) and P. aeruginosa (ATCC® 27853TM) acquired from the ATCC cell bank, similarly to method presented by [46,53,54]. The cylindrical samples (4 cm in diameter and 2 mm thick for pastes and 2.6 cm in diameter for mortars) were exposed to ultraviolet light (λ = 360 nm) for 24 h in a chamber with a lamp at 10.3 Wm−2 intensity prior to the test with bacteria, similar to [54,55]. The antimicrobial activity test on cement mortars irradiated with the UVA light shortened the inactivation time of the bacteria and, additionally, it was possible to compare them with the action of natural daylight [53,54,55]. Afterwards, each bacterial inoculum was added to LB agar at 37 °C, and was homogenized and served in Petri dishes; then, the material to be evaluated (paste or mortar) was placed in the center of the box and left in a flow cabinet until gelling. It was incubated for 18 h at 37 °C. After incubation, each plate was examined and visualized for the presence of colonies grown on the surface of the material or the formation of inhibition halos was registered. The culture medium and supplements used were BHI Broth (Becton Dickinson, Franklin Lakes, NJ, USA), Luria Bertani Agar (Becton Dickinson, Franklin Lakes, NJ, USA), saline solution (Corpaul, Medellín, Colombia), and saline phosphate buffer (Bio-Connect, Huissen, The Netherlands). A Sensi-disc control of gentamicin was used (6 mm in diameter and 2 mm thick).
3. Results and Discussion
3.1. Raw Materials
3.2. Characterization of the CW-OPC Hybrid Pastes
3.3. Effect of TiO2 and ZnO Particles in Mechanical and Photocatalytic Properties
3.4. Biological Activity with Bacteria
- The contribution of amorphous and soluble silica from SS is an essential component to achieve compressive strengths in pastes above 10 MPa. A high sodium content in the mixtures reduces the viscosity of the pastes and results in carbonation reactions with the environment, which can generate efflorescence due to carbonated products on the surface of the samples. The formation of the CASH gel and the hybrid N-CASH gel was evidenced by the CW-OPC mixture. The optimal molar ratio values for the preparation of pastes with strengths of 40 MPa at 28 days were 7.7 for SiO2/Al2O3 and 0.12 for Na2O/SiO2.
- In the evaluation of the capacity of alternative silicate formation, the replacement of SS by 50% glass was not beneficial due to the poor dissolution of the glass at room temperature and under the alkaline conditions studied. Additionally, the incorporation of glass as a fine aggregate decreased the compressive strengths. The values obtained were 25.21, 11.57, and 9.08 MPa at 28 days of curing for the MRef mortar (made with river sand), M11-SS mortar, and M11-50SS:50G mortar using G as a fine aggregate, respectively. The loss of strength was attributed to the formation of a weakened aggregate−paste transition zone with a high porosity and the formation of microcracks around the glass aggregate.
- The 100SS-5Z and 50G:50SS-10Ti pastes showed an effective photocatalytic activity for Rh-B degradation, with percentages of Rh-B degradation of 98.4% and 76.4%, respectively, after 24 h, but problems of mixing and poor dispersion of the nanoparticles were observed and could be the main technological challenge.
- The 100SS-5Z and 50G:50SS-10Ti pastes, together with their respective mortars, were effective at inhibiting the growth of P. aeruginosa and K. pneumoniae strains, evidenced by the formation of bacterial inhibition halos around the sample discs.
- These results demonstrated the possibility of using ceramic tile waste in high proportions for the elaboration of new rendering mortar with innovative properties.
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
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|LOI, 1000 °C||0.6||4.10||1.46|
|Mixture||Dry Density, kg/m3||Apparent Density, kg/m3||Porosity, %||Water Absorption, %|
|M9||1820 ± 10||2520 ± 10||28 ± 0.38||15.3 ± 0.2|
|M11||1870 ± 20||2430 ± 10||23 ± 0.36||12.2 ± 0.2|
|M11-SS||1870 ± 20||1880 ± 10||1900 ± 10||1920 ± 10||1970 ± 10|
|M11-50SS:50G||-||1990 ± 10||2040 ± 20||2040 ± 30||2040 ± 20|
|Mixture||C/Co after 24 h||Degradation of RhB, %|
|Type||Mixture||Formation of Bacterial Inhibition Halos|
|K. pneumoniae ATCC||P. aeruginosa ATCC|
|Sensidisc whithout antibiotic||No||No|
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Bonilla, A.; Villaquirán-Caicedo, M.A.; Mejía de Gutiérrez, R. Novel Alkali-Activated Materials with Photocatalytic and Bactericidal Properties Based on Ceramic Tile Waste. Coatings 2022, 12, 35. https://doi.org/10.3390/coatings12010035
Bonilla A, Villaquirán-Caicedo MA, Mejía de Gutiérrez R. Novel Alkali-Activated Materials with Photocatalytic and Bactericidal Properties Based on Ceramic Tile Waste. Coatings. 2022; 12(1):35. https://doi.org/10.3390/coatings12010035Chicago/Turabian Style
Bonilla, Ashley, Mónica A. Villaquirán-Caicedo, and Ruby Mejía de Gutiérrez. 2022. "Novel Alkali-Activated Materials with Photocatalytic and Bactericidal Properties Based on Ceramic Tile Waste" Coatings 12, no. 1: 35. https://doi.org/10.3390/coatings12010035