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RESEARCH Mechanical and microstructural characterization of cement mortars prepared by waste foundry sand (WFS) Sinem Çevik1 & Tugba Mutuk1 & Başak Mesci Oktay1 & Arife Kübra Demirbaş1 Received: 22 February 2017 /Revised: 1 June 2017 /Accepted: 15 June 2017 # Australian Ceramic Society 2017 Abstract Foundry sand is used spent in sandmolds of ferrous and non-ferrous industries. When it is no longer used, it has become solid wastes generated by foundries. According to European Union regulations, it is a non-hazardous waste so it can be recycled in other industries, especially in cement industry. In the present paper, the mechanical properties and characterization of cement mortars are prepared by using waste foundry sand coming from Turkey steel manufacturer as partial replacement of natural sand were experimentally investigated and the possibility of using waste foundry sand (WFS) instead of natural sand in mortar has been determined. Recycling of solid foundry waste is considered as an environ- mentally friendly alternative to solve the problem of disposing of the solid wastes. Cement mortar admixtures were prepared by using with variable percentages ofWFS ranging from 15 to 60%. Additionally, to make comparison, one reference admix- ture sample was fabricated without using any waste foundry sand. The effect of WFS on the compressive strength of the cement mortar was analyzed. The compressive strengths values of all the specimens were recorded for 3, 7, and 28 days and results showed that when the amount ofWFS replacement is increased, the strength decreased slightly according to the comparison of the reference sample. However, cement mortar containing 15% additive has showed the highest strength val- ue at 3 and 28 days. As a result in the present study, it is observed that optimum additive amount of WFS as replace- ment of natural sand in cement mortar is 15%. SEM images were also taken to evaluate the relationship between micro- structure and strength of the specimens. Moreover, scanning electron microscope (SEM) examination was carried out to explain the effectiveness of the matrix in the reuse of WFS. Microstructural observation of the samples by SEM showed that the sand particles of the WFS were well embedded in the cementitious matrix. Keywords Cementmortar . Mechanical treatment . Microstructure .Waste foundry sand Introduction Industrialization is a key factor for any developing economy. However, it leads to serious environmental problems from a different point view. Therefore, industrial wastes become a by- product of growth [1, 2]. Turkey is a fast-growing, develop- ing, and progressing country. Growth in economy and produc- tion, urbanization, increase in population, and economic wel- fare rising bring about ever-increasing waste production. To control the excess amount of waste, the fabrication process should be completed without production of these waste mate- rials or with as low as possible amount of it. Also, recycling and ultimately disposal of waste most accurately with regard to an economy and environment should be done [3]. Usually, the industrial by-products are either stored or land- filled without known detrimental effects on the environment. The use or recycling of these byproducts has become a world- wide interesting research topic, due to the increasing concerns about the environment, natural resources consumption, limit- ed landfill space, and rapidly increasing disposal cost. Turkey casting sector occupies a prominent place among the other various industries in Europe and the world. Turkey is fourth leading European producer with Spain after Germany, * Sinem Çevik sinemu@omu.edu.tr 1 Faculty of Engineering, Department of Materials Science and Engineering, Ondokuz Mayis University, Kurupelit, 55139 Samsun, Turkey J Aust Ceram Soc DOI 10.1007/s41779-017-0096-9 Italy, and France. 80% of the production of Turkey casting industry is used for several industries, e.g., automobile, trac- tor, truck, white goods, defense, and construction. The casting craft exists in Anatolian territories for 5000 years. Casting is hard and labor work. It is a B4D^ industry which means that dirty, dusty, difficult, and dangerous. However, it is one of the most essential sectors in the world, both providing employ- ment and contribution to the national economy [4]. Therefore, Turkey and Europe need to have modern and developing cast- ing industries. The primary waste of casting industry is natural silica sand. Turkey casting sector expects that establishing legal obliga- tions and supports providing the reuse of this sand in other industries (cement, asphalt, road construction, and ready mixed concrete manufacturing, etc.,) like in EU and the USA.Moreover, the other expectation is about providing con- venience in the building of storage facilities for not reusable ones. Waste management has gradually become important in foundries regarding ecology, economy, and environment since solid waste management in the steel industry are broadly clas- sified in B4 Rs,^ i.e., reduce, reuse, recycle, and restore the materials [5, 6]. Because foundry management is not a clean production method, the processes used in the production of casting in our country generate 450,000 tones of waste. The amount of this consists of approximately 65% sand, 10% slag, 15% clay dust, and 10% refractor, oil, stone, dye, etc. Foundry sand (FS) which is a byproduct of the ferrous and nonferrous metal casting industry, where sand has been used for centuries as a molding material because of its unique engi- neering properties. Approximately 100 million tons of foundry sand is used in the casting manufacturing process, and 4–7 million tons are discarded annually [7]. This kind of discarded material can be utilized for aim to recycle. Waste foundry sand (WFS) can be used for economic and sustainable development in different industries, mainly cement and concrete industry. Foundry sand has very high silica content approximately 93– 95% like natural sand that we used in cement mortar and con- crete. For this reason, WFS can be a replacement with different percentages of aggregate or natural sand in cement and con- crete [8, 9]. Devi et al. [10] researched that utilization of waste foundry sand in geo-polymer concrete. With the addition of waste foundry sand in geo-polymer concrete compressive and tensile strength has been increased. Siddique et al. [11] inves- tigated the use of WFS in concrete manufacturing. WFS have been used as a partial replacement of fine aggregates of the concrete. Test results showed that water absorption capacity of the concrete decreases with increasing WFS content. Compressive strength results of additionWFS in concrete mix- tures were increased on control samples. Smarzewski et al. [12] studied of influencing of all the tested concrete properties with additions of coal cinder (CC) and waste foundry sand (WFS) and the result of CC and WFS improves resistance to salt crystallization and freezing in concrete. The primary aim of this study is to comprehend the possi- bility of the recycling of WFS coming from Turkish steel industry in other industries, especially in cement manufactur- ing. By this purpose, cement mortars with the admixture of WFS were evaluated by mechanical tests. SEM and EDS mapping were also used to analyze the microstructure of ce- ment mortars. These cement mortars consist of WFS as a partial replacement of natural sand. Therefore, the relationship between foundries and cement industry in Turkey could be enhanced to solve the disposal of solid waste, to execute solid waste management properly, and to decrease the environmen- tal problems. Materials and method Materials Cement is mainly used as a binder for concrete and mortar. Cement is a hydraulic-setting material. It consists of finely ground, non-metallicinorganic compounds. Cement is produced by grinding cement clinker and othermain orminor constituents. When water is added to cement, a cement paste is formed which sets and hardens with the help of hydration reactions. After hardening, it retains its strength and stability even under water. Portland cement is one of the most widely used binder materials to prepare concrete [13]. It is composed of 95– 100% of clinker as a main constituent. Cement clinker is made of a raw material mixture that is added to the cement kiln and sintered at a temperature of 1400 °C. The basic materials to produce cement clinker have to consist of calcium oxide (CaO), silicon dioxide (SiO2), and small amounts of alumi- num oxide (Al2O3) and iron oxide (Fe2O3). Rawmaterials that have these properties are limestone or chalk and clay or lime- stone as its natural occurring mixture. In this study, the commercial Portland cement type CEM I 42.5 R corresponds to the 42.5 standard compressive strength classes with high initial strength development (R) in accordance with TS EN 197-1:2012 is used. The chemical composition and the result of XRF analysis of cement are shown in Table 1. Table 1 Chemical composition of cement (%) Chemical composition OPC SiO2 19.95 Al2O3 4.52 Fe2O3 3.46 CaO 62.74 MgO 1.41 SO3 2.88 Loss on ignition 3.26 OPC ordinary portland cement J Aust Ceram Soc WFS is a mixture of high-quality size-specific silica sand, few amount of impurity of ferrous and nonferrous by-products from the metal casting process itself, and a variety of binders. In the casting process, molding sands are recycled and reused multiple times, and small residues of ferrous and non-ferrous byproducts often come from the recycling process. Before it is reused, silica sand needs to be cleaned using screening sys- tems and magnetic separators to segregate reusable sand from other wastes and to separate particles of varying sizes. Although WFS is partially a recycled material itself and suc- cessfully recycled/reused through many production cycles, after many times it loses its characteristics such as the clean- liness and the uniformity. When the material became unsuit- able for the more manufacturing cycles, it is discarded as waste product [9, 14–16]. WFS used in this research were used as multiple times. According to the European Union and National regulations, it is classified as a non-hazardous waste. The classification and the behavior of foundry sand strictly depend on the type of casting process and the industry sector from which it originates, and especially from the type of bind- er systems used in the process. Typically, two types of binder systems, with different physical and environmental character- istics, are used: clay and chemical binder. Accordingly, found- ry sand is categorized as clay bonded system (green sand) and chemically bonded system. The most commonly used one is Green sand. Chemically bonded sand consists of silica sand and chemical binder that is activated by a catalyst. Chemically bonded sands include 93–99% silica and 1–3% chemical binder [9, 15]. The chemical composition of the foundry sand is directly related with to the metal which molded at the foundry. Molded metal determines the binder that was used, as well as the combustible additives. It also can impact its performance. Waste foundry sand consists primarily of silica sand, coated with a thin film of burnt carbon, residual binder (bentonite, sea coal, resins), and dust [17] The WFS used in the present study is chemically bonded sand coming from the steel casting molding process of a Turkish steel foundry which serves several industries like en- ergy, railway, cement, heat treatment, and work machinery. TheWFS was chemically characterized in terms of specific weight, and X-ray fluorescence (XRF) analysis results are shown in Table 2. Cement mixture proportions Standard sand and WFS were analyzed by sieving before the experimental work was started. After sieve analysis, the values appeared are tabulated below (Table 3). Fineness mod- ulus was calculated according to the results obtained in Table 3. Table 2 Chemical composition of WFS (%) Chemical composition WFS SiO2 86,32 Al2O3 1.59 Fe2O3 1.89 CaO 0.17 MgO 3.56 Na2O 0.09 K2O 0.31 WFS waste foundry sand Table 3 Sieve analysis and particle size of standard sand and WFS Sieve size (μm) WFS weight retained (g) WFS weight retained (%) WFS cumulative retained (%) Standard sand weight retained (g) Standard sand weight retained (%) Standard sand cumulative retained (%) 800 350 8.92 8.92 914.5 67.98 67.98 500 2327 59.3 68.22 169.6 12.61 80.59 300 984.3 25.1 93.32 98.2 7.3 87.89 200 163.5 4.17 97.49 32.4 2.41 90.3 100 73.6 1.88 99.37 108.5 8.07 98.37 Pan 23.3 0.59 100 21.9 1.63 100 Total 3921,7 467.32 1345.1 525.13 Table 4 Mixture proportions of the mortar Mix. symbol WFS (%) Cement (g) Sand (g) WFS (g) R 0 450 1350 – F1 15 450 1147.5 202.5 F2 30 450 945 405 F3 45 450 742.5 607.5 F4 60 450 540 810 WFS waste foundry sand J Aust Ceram Soc Fineness modulus of WFS ¼ ∑Cumulative retained %ð Þ . 100 →4:67 Fineness modulus of standard sand ¼ ∑Cumulative retained %ð Þ . 100→5:25 0,000 0,005 0,010 0,015 0,020 0,025 0,030 0,035 0,000 0,005 0,010 0,015 0,020 0,025 0,030 0,035 0 2 4 6 8 10 12 14 16 18 20 22 0 2 4 6 8 10 12 14 16 18 20 22 Strain (mm/mm) S tr e s s ( N /m m 2 ) m m/ N( s s ert S 2 ) Strain (mm/mm) R-3 days 0,00 0,01 0,02 0,03 0,04 0,05 0,00 0,01 0,02 0,03 0,04 0,05 0 5 10 15 20 25 0 5 10 15 20 25 Strain (mm/mm) S tr e s s ( N /m m 2 ) m m/ N( s s ert S 2 ) Strain (mm/mm) F1-3days 0,00 0,01 0,02 0,03 0,04 0,05 0,00 0,01 0,02 0,03 0,04 0,05 0 5 10 15 20 25 0 5 10 15 20 25 Strain (mm/mm) S tr e s s ( N /m m 2 ) S tr e s s ( N /m m 2 ) Strain (mm/mm) F2-3days 0,00 0,01 0,02 0,03 0,04 0,05 0,06 0,00 0,01 0,02 0,03 0,04 0,05 0,06 0 2 4 6 8 10 12 14 0 2 4 6 8 10 12 14 Strain (mm/mm) S tr e s s ( N /m m 2 ) S tr e s s ( N /m m 2 ) Strain (mm/mm) F3-3 days 0,000 0,005 0,010 0,015 0,020 0,025 0,030 0,035 0,040 0,000 0,005 0,010 0,015 0,020 0,025 0,030 0,035 0,040 0 2 4 6 8 10 12 14 16 0 2 4 6 8 10 12 14 16 Strain (mm/mm) S tr e s s ( N /m m 2 ) S tr e s s ( N /m m 2 ) Strain (mm/mm) F4-3 days Fig. 1 R and 15, 30, 45, and 60% WFS adding samples 3 days strain-stress graphs J Aust Ceram Soc It is found that the fineness modulus of standard sand is 5.25. It means the average value of standard sand is in between the fifth sieve and sixth sieve. Therefore, the average standard sand size is in between 500 μm and 800 μm. The same cal- culations are applied to WFS. The fineness modulus of WFS is found as 4.67. It shows the average WFS size is in between 300 and 500 μm. The mixture was designed based on TS EN 2009 [18]. Each mixture consists of 1350 kg/m3 sand, 450 kg/m3 ce- ment, and 225 ml of water and also water to binder ratio, 0.5 was used. Waste foundry sand was added as a replace- ment of sand and the proportion of WFS for the mortar as shown in Table 4. R series were prepared as control sam- ples. F series show that WFS was added at the different ratio in the mortar. Compressive strength The cubes mold sizes of 40 mm × 40 mm × 40 mmwereused for compressive strength tests. All the molds were cleaned and oiled properly. WFS were used as a partial replacement of sand in the mortar. After preparing the mortar of mixture, all samples were cured for 3, 7, and 28 days. The compressive tests were conducted with a 10-tone universal MARES tension-compression test unit. Microstructural characterization Particularly, cementitious materials exhibiting microstructural heterogeneities may provide different chemical environments within the matrix. Thus, it has been realized in the past years that solutions for large-scale problems, such as metal contam- inants in the environment, remediation, and the storage of radioactive waste, should also be based on detailed informa- tion on the micro-scale. Highly heterogeneous cementitious materials can be ana- lyzed by a variety of analytical techniques, such as X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). These methods are well suited to identify different mineral phases and to gain spatially resolved information on the mineralogical composi- tion, the morphology of the cementitious material, and ele- mental distributions [19, 20]. The microstructural characterization and EDS chemical mapping of samples were observed by a JEOL 7001F Field Emission (FE) Scanning Electron Microscope with an EDX attachment which has an 80mm2 X-MAX detector. Elemental maps are generated by scanning the sample with the X-ray beam at a selected energy and correspond to qualitative ele- mental distribution. The micro-images are taken by fractured surfaces of cement mortars after mechanical testing. Before the observation, all the samples were coated with gold sputtered to make the surface conductive for surface topogra- phy examinations. After the microstructure analysis, the SEM system would not be configured to take a backscatter electron image (BSE) to carry out EDS elemental mapping. EDS map allows a more accurate analysis in BSE mode. Moreover, a reliable set of chemical composition data is the key to a precise and accurate analysis. However, an important disadvantage of EDS is that the signal is collected from a volume of sample, several mi- crons in size depending on the electron energy. It can be called an interaction volume. Because of that, the proximity of epoxy resin or other particles of different chemical composition af- fects the measurement and adds noise and uncertainty to the spatial resolution. Therefore, the EDS was performed on frac- tured surface specimens taken from the inner surfaces of the samples. 0,00 0,01 0,02 0,03 0,04 0,05 0,00 0,01 0,02 0,03 0,04 0,05 -5 0 5 10 15 20 25 30 35 40 -5 0 5 10 15 20 25 30 35 40 Strain (mm/mm) S tr e s s ( N /m m 2 ) S tr e s s ( N /m m 2 ) Strain (mm/mm) R F1 F2 F3 F4 Fig. 3 Effect of different percentage WFS on compressive strength after 28 days 0,00 0,01 0,02 0,03 0,04 0,05 0,00 0,01 0,02 0,03 0,04 0,05 0 5 10 15 20 25 0 5 10 15 20 25 Strain (mm/mm) S tr e s s ( N /m m 2 ) S tr e s s ( N /m m 2 ) Strain (mm/mm) R F1 F2 F3 F4 Fig. 2 Effect of different percentage WFS on compressive strength after 3 days J Aust Ceram Soc Results and discussion Mechanical strength analysis WFS, a kind of waste, were added as a replacement of sand in cement mortar and then these samples’ mechanical treatment and microstructure were analyzed by using compressive strength test and scanning electron microscopy (SEM) tech- nique respectively. 15, 30, 45, and 60% WFS were added to mortar instead of sand. Samples were cured for during early age strength 3 and 7 days and late age strength 28 days for the compressive strength test. R denotes control sample, and F denotes WFS added at the different ratio in the mortar. 15% added sample is F1, 30% added sample is F2, 45% added sample is F3, and 60% added sample is F4. These samples after mechanical testing 3 days strain-stress graphs as shown in Fig. 1. As seen in the graphs, 15 and 30% WFS adding samples were compared to the reference sample almost gave the higher result. 45% and more added foundry sand were decreased in the early age strength (3 days) of the samples. The maximum compressive strength of the samples for 3 days was compared with each other in Fig. 2. The highest compressive strength values of R, F1, and F2 samples were 19.83, 22.51, and 22.28 MPa, respectively. We can see the same result in Fig. 1. As seen in Fig. 3, compressive strength was measured at the ages of 28 days. They concluded that partial replacement of sand with WFS caused considerable reduction in late age strength. The highest compressive strength values of R and F1 samples were 35.04 and 33.13 MPa, respectively. These results are very approximate values. But F3 and F4 samples were observed that decreased the compressive strength. On the other hand, compared to the reference samples, 15% WFS added samples gave the convenient result for the Fig. 4 a SEM micrographs of reference samples of cement mortars. b 15 wt% WFS added sample after 28 days curing time J Aust Ceram Soc standards limits [21]. As a result, WFS can be used as recy- clable waste. Microstructural analysis Portland cement is mainly composed of calcium silicates (tri- calcium silicate, C3S, and di-calcium silicate, C2S), which react with water during the hydration and produce calcium silicate hydrate and calcium hydroxide, providing high strength and alkalinity to the material, respectively [22]. SEM images obtained from cement mortars with WFS (Fig.4) after 28 days curing shows calcium hydroxide (CH), also known by its mineral name portlandite. Calcium hydrox- ide forms as crystals with a wide range of shapes and sizes as shown in Fig. 4.a to the reference sample. CH structure chang- es to the calcium silicate hydrate (C-S-H) gel structure with the addition of WFS. This result is consistent with previous finding of Saleh et al. [23]. This structure has beneficial effects on the strength and permeability. C-S-H gel structure respon- sible for the strength in cement-based materials and also it seems like a spider web (Fig. 4b). There was not seen highly localized porosity in the ages that were studied because of the structure of ettringite. In Fig. 4a, the hydration product of ettringite as a short needles form can also be seen. Ettringite is the mineral name for calcium sulfoaluminate (3CaO·Al2 O3· 3CaSO4·32H2O). This structure is normally found in portland cement concretes. Because of the needle-like structure, it pro- vides a decrease in the pore structure. However, it does not contribute to too much strength to structures. The formation of ettringite could be indicated from Al-rich regions of elemental mapping. Energy dispersive microanalysis (EDS) mapping has been used to determine the elemental distribution of chemical ele- ments inherent to the cement matrix in hardened cement paste. The following elements were observed from the spectra: Si, Ca, O, Al, C, Mg, and Fe. The distribution of elements, by EDS analysis, (shown in Fig. 5) shows that Ca and Si are mainly concentrated in the crystals, Si is uniformly distributed throughout the material, and O also seems to be uniformly distributed. Al map illustrates highly enriched regions. The microscopic investigations indicate cement-derived el- ements Ca, Si, Al, Fe, and C which is in high amount predicting coming from WFS in the cement matrix. The Ca distribution mainly reflects zones of unhydrated clinker and hydrated cement minerals. The highly concentrat- ed Ca regions indicate the presence of mainly calcium silicate hydrates, C-S-H, and clinker minerals.Regions with less Ca indicate the formation of C-S-H and portlandite (Ca(OH)2). In this study, EDS mapping was used to see the correlation between the microstructure and mechanical properties during the recycling of waste foundry sand in cement mortars. The technique here allows a quick visual determination of micro- structures of different hydrated and unhydrated chemical Fig. 5 Visual representation of the distribution of elements measured by EDS J Aust Ceram Soc components formed by complex materials and where they are formed predominantly in the whole structure. Therefore, the microstructure shown in Fig. 6 is the entire field of view. Also, elemental mapping was used only to give a qualitative image of the distribution of elements of the sample in this study. Energy-dispersive X-ray spectroscopy (EDS) and elemental mapping have traditionally been used to characterize elemen- tal composition and spatial distribution to understand and de- sign for materials properties, not like XRD which have been used to add the phase component to the analysis. Also, flexible stage controls and sample holders allow finished ceramic parts in their native state to be analyzed even if they are irregularly shaped. However, according to the capability of SEM device, sometimes elemental mapping fails to provide the complete data set required to fully understand the sample composition. In Fig. 6, qualitative EDS mapping of these cement include Ca and Al and also the presence of C, minor quantities of Mg, and major quantities of Si, suggesting calcium mono- carboaluminate intermixed with other solids. To summarize, from a mechanical and microstructural point of view, the high level of replacement of regular sand by WFS in portland cement matrices showed no certain ad- vantages. However, portland cement has been proved to be a suitable matrix to prepare mortars for recycling of waste foundry sand in the optimum level of replacement, below 20%. When ordinary portland cement as a binding matrix was used with WFS addition, the compressive strength was not decreased. In all cases, the minimum strength require- ments for landfilling (1 MPa) were well complied with [24]. Electron microscopic (SEM/EDX) analysis consistently showed that the matrix was compact with barely any pores, which would largely explain its good mechanical performance. Conclusions The scope of this study, the possibility of using waste foundry sand as a partial replacement of natural sand in cement mortar was experimentally investigated. Mechanical strength (late age strength 28 days) of mortar decreased with the increase in sand replacement with different replacement values of WFS. But, the compressive strength results with 15 and 30%WFSmortars increased up to 22.51 and 22.28MPa when compared to control mortar mixture (19.83 MPa) without WFS at 3 days. All strength results in this study are acceptable for the TS EN standards. Moreover, the image of the required microstructure was also observed by SEM/EDS analyses. Fig. 6 EDS pattern of cement mortars having 15 wt% WFS addition after 28 days curing time J Aust Ceram Soc Microstructural evaluation of fractured surfaces provided the morphological information that was related to the mechanical performance obtained from tensile-compression tests. This kind of wastes such as WFS coming from steel industries is not commonly used in the cement-concrete industry, especial- ly in Turkey. The present study represents a suitable solution to the environmental impact of several industrial activities and open opportunities for giving value to the wastes. Therefore, such materials can be utilized in the cement-concrete industry properly. This study’s results provide a preliminary work for WFS recycling because there are not many studies about this topic. In future studies, the use of WFS in concrete industry will be investigated. Acknowledgements We would like to acknowledge Yunus Gedik for the assistance with the sample preparation and observation for SEM/EDS analysis. We gladly acknowledge that SEM/EDS analysis was performed at KİTAM, Karadeniz Advanced Technology and Research and Application Center. We also acknowledge Director of Yesilyurt Iron Steel Vocational High School of Assoc. Prof. Kemal Yıldızlı for the assistance with EDS mapping analysis. References 1. Joshi, R.: Effect of using selected industrial waste on compressive and flexural strength of concrete. 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Navarro-Blasco, I., Fernández, J.M., Duran, A., Sirera, R., Álvarez, J.I.: A novel use of calcium aluminate cements for recycling waste foundry sand (WFS). Constr Build Mater. 48, 218–228 (2013) J Aust Ceram Soc Mechanical and microstructural characterization of cement mortars prepared by waste foundry sand (WFS) Abstract Introduction Materials and method Materials Cement mixture proportions Compressive strength Microstructural characterization Results and discussion Mechanical strength analysis Microstructural analysis Conclusions References
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