Template for Electronic Submission to ACS Journals The Journal of Engineering Research (TJER), Vol. 16, No. 1 (2019) 53-62 DOI: 10.24200/tjer.vol16iss1pp53-62 DEVELOPMENT AND EVALUATION OF CERAMIC TILES USING WASTES AND SOLID MINERALS Z.U. Elakhame *,a , Y.L. Shuaib-Babata b , and I.O. Ambali c a Department of Prototype Design and Development, Federal Institute of Industrial Research, Lagos, Nigeria. b Department of Materials and Metallurgical Engineering, University of Ilorin, Ilorin, Nigeria. c Department of Materials and Metallurgical Engineering, University of Ilorin, Ilorin, Nigeria. ABSTRACT: This paper focuses on the need for domesticating the production of building materials like tiles to address the problem of Nigeria over dependence on imported goods, despite adequate availability of mineral resources like clay, quartz and feldspar in the country. Clay, quartz and feldspar, and milled glass were respectively obtained from Ogijo in Ogun State, Okpila in Edo State and Oshodi, Lagos State of Nigeria were characterized using ASTM C71 as a guide. Samples of the ceramic tile were produced from varying mixtures of clay, quartz, feldspar and milled glass. The chemical and physio-mechanical properties of the samples were also determined. The results showed that the clay sample belong to Alumino-silicate group with 59.20% silica and 21.25% alumina. The samples’ properties met the required standards; hence, the materials were found suitable for production of ceramic tiles of acceptable standards. Though, the porosity of the sample tiles increased as the percentage weight of the clay material in the mixture decreased the proportion of quartz, feldspar and milled glass increased. The sample containing 70% Clay and 30% Feldspar had better formulation properties than others. Keywords: Apparent porosity; Bulk density; Ceramic; Tile; Milled glass; and Solid minerals. باستخدام النفايات واملعادن الصلبة الفخاري بالط السرياميكالوتقييم انتاج ، .يو. االخاميد ز *أ اتاباب بشعي .ال .واي ب اليبام .ه وأى. او ج على السلع ريبالكنيجرييا اعتماد مشكلة لحل حمليا تركز الدراسة على احلاجة إىل إنتاج مواد البناء مثل البالط: امللخص الطني وقد حصلنا على. يف البالد سيليكات االلومنيومتوافر املوارد املعدنية الكافية مثل الطني والكوارتز ورغم املستوردة والية اوكيال يف منطقة و اوغن والية يفأوجيو منطقةوالزجاج املطحون على التوالي من سيليكات االلومنيوم والكوارتز و بإنتاج عينات من بالط و قمنا كدليل. سي 7 استيم يف نيجرييا باستخدام الغوس اوشودي يف والية منطقةايدو و بتحديد اخلصائص قمناوالزجاج املطحون. كما االلومنيومسيليكات والكوارتز والسرياميك من خليط من الطني أظهرت النتائج أن عينة الطني تنتمي إىل جمموعة ألومينو سيليكات قد و .الكيميائية والفيزيائية امليكانيكية للعينات املواد دنا ان وجاستوفت خصائص العينات املعايري املطلوبة ؛ وبالتالي ، وقد . ألومينا ٪92.90سيليكا و 02.95بنسبة البالطات قد ازدادت مع اخنفاض عينة على الرغم من ذلك ، فإن مسامية. و مناسبة إلنتاج بالط السرياميك باملعايري باملقبولة وكان والزجاج املطحون. سيليكات االلومنيوم النسبة املئوية لوزن املادة الطينية يف اخللطة املختلطة وزادت نسبة الكوارتز و .أفضل من غريها تكوينخصائص سيليكات االلومنيوم من ٪ 05الطني و من ٪ 05حتتوي على اليت عينة لل املعادن الصلبة.؛ الزجاج املطحون ؛ البالط ؛ سرياميكال ؛الرئيسة الكثافة ؛الظاهرة املسامية مفتاحية:الكلمات ال *Corresponding author’s e-mail: ezeberu@yahoo.com The Journal of Engineering Research (TJER), Vol. 16, No. 1 (2019) 53-62 1. INTRODUCTION In Nigeria, natural mineral resources, such as clay, feldspar, quartz are available in large quantities Shuaib-Babata and Mudiare (2017), but the country is still highly being challenged with economic problems. Some studies have attributed the present Nigeria economic problem to over-dependence on foreign goods, oil and gas and to negligence of other sectors (Chete et al. 2017; Projectsxtra 2017; Shuaib- Babata et al. 2017a). It is claimed that an identified veritable tool towards any nation development is Industrialization (Shuaib-Babata et al. 2017b; Shuaib-Babata et al. 2017c). Availability of mineral resources in Nigeria has been the backbone of the nation’s economic and industrial development aspirations Foraminifera (2017). Presently, there are several calls for diversification of Nigeria’s economy and significant reduction of its overdependence on oil and gas to come out permanently of the present economic recession Foraminifera (2017). Production capacity from locally available raw materials used in development of technology in the transformation of the raw materials to finished products is a significant factor towards a successful industrialization (Shuaib-Babata et al. 2017a, Shuaib- Babata et al. 2017b). The identified bases for the development of any industrial sector include access to raw materials, labor force, funds and technology Hughes (2008). Effective industrialization could be significant to reduce overdependence of a nation on foreign goods and enhance export base Shuaib- Babata et al. (2017a). Worldwide, production and consumption of ceramic tiles has recently increased all over the world as result of rapid development of real estate industry WIFI Ceramics (2017). The tiles used in the estate development are of different quality; it ranges from high to middle and low quality, which is imported to Nigeria, especially from China. With the present call for economic diversification in Nigeria, the need for local production of ceramic tiles with good quality is highly essential. This will be of help to proffer a solution to the problem and sustain the country economy through industrialization. There have been numerous attempts to utilize either industrial or agricultural wastes in the manufacture of wall and floor ceramic tiles in the past last two decades (Elakhame et. al. 2016; Cesar et al. 2011; Juan, et al. 2010). Industrial wastes are considered to be an important part of the materials used. Cement kiln dust (CKD) as a great trouble maker waste, was utilized in ceramic tile bodies by Youssef (2002), to replace half the feldspar required for ceramic wall tile body with a double target of cost reduction and environment protection. In that study, verification parameters of the fired samples was measured and the water absorption was within both ISO and Egyptian standards limits of wall tiles. CKD in the mixture makes it less dense, more porous and lowers the compressive strength (Safiuddin et al. 2010; Yoshizawa et al. 2004; Central Pollution Control Board (CPCB), 2000; Torgal and Jalali 2010). For better quality tiles, the basic raw materials employed for the production of ceramic tiles include quartz and feldspar (which serve as a source of silica and alumina to give the tiles the desired strength) and clay from a good source to serve as binder. In this study, milled glass and aluminum were considered as a primary source of alumina and silica. This study aims at the development of standard composite ceramic tiles-based (CCT) using available mineral resources and wastes to aid local production of building materials in Nigeria. It also focuses on the use of cheaper and durable materials to fabricate the CCT to enhance its properties by variation of fillers to identify the best mechanical and physical properties of the produced tiles. In the end, this should assist in solving the problem of unemployment among youths. It should also help in diversification of economy and solve the problem of over dependence on the oil and gas sectors, which had led to economic recession in the country. 2. MATERIALS AND METHODS 2.1 Materials In this study, the major materials used include clay (CY), quartz (QZ), Feldspar (FR) and milled glass (MG). The clay material and the milled glass bottle was sourced from Ogijo-Shagamu Area, Ogun State and Oshodi, Lagos Nigeria respectively. The quartz and feldspar were obtained at different deposits in Okpila, Edo State, Nigeria. Samples of the raw materials for the production of ceramic tiles in solid forms are shown in Fig 1. 2.2 Methods 2.2.1 Chemical Analysis The chemical compositions of the representative samples of the clay, quartz, feldspar and milled glass were determined at Engineering Materials Development Institute (EMDI), Akure, Nigeria using Atomic Absorption Spectrometer (AAS) UNICAM 929. This is in line with the data reported by (Ryan 1978; Yoshizawa et al. 2004; and Safiuddin, et al. 2010). Clay Feldspar Quartz Glass Bottles Figure 1. Samples of the raw materials used for the production of ceramic tiles. 54 Z.U. Elakhame, Y.L. Shuaib-Babata, and I.O. Ambali 55 2.2.2 Preparation of Materials 2.2.2.1 Clay Materials To remove debris and other unwanted materials in the clay sample, the clay was soaked in water for five (5) days, sieved with a mesh of 350µm and dried at room temperature for one week (7 days). Subsequently, the dried sample was milled and sieved into 100 µm sizes in line with the practice of Elakhame et al. (2016b). 2.2.2.2 Quartz, Feldspar and Milled Bottle. The quartz and feldspar and the milled glass bottle (additive materials) were crushed using a Hammer Milling Machine (Model; 000T, PUISSANE; 1.5KV, S/N; 13634) and milled into fine size particles using ball-milling machine (Model; 87002…. Limoges-France, Type; A50---43), and then sieved with a Vibro-Sieve (Model; Fritsch GmbH, D- 55743.1 Dar-Oberstein Germany) into 100 µm particles size. 2.3.2 Raw Materials Mixtures In forming the raw materials mixtures for the production of ceramic tiles, milled bottle, quartz and felspar were added to the clay materials at different proportion as presented in Table 1 (a & b). Table 1a. Proportion of clay and other materials in forming the raw mixes for the production of ceramic tiles (Formulation A – C). Samples Sample Formulation A Sample Formation B Sample Formation C CY (%) QZ (%) CY (%) FR (%) CY (%) MG (%) 1 100 0 100 0 100 0 2 80 20 80 20 80 20 3 70 30 70 30 70 30 4 60 40 60 40 60 40 5 50 50 50 50 50 50 6 40 60 40 60 40 60 7 30 70 30 70 30 70 8 20 80 20 80 20 80 Table 1b. Proportion of clay and other materials in forming the raw mixes for the production of ceramic tiles (Formulation D. FORMULATION SAMPLE D CY (%) QZ (%) FR (%) MG (%) 50 0 40 10 50 10 30 10 50 40 0 10 50 5 5 40 0 35 35 30 Note: Clay = CY, Quartz = QZ, Feldspar = FR, and Milled glass = MG 2.3.3 Tiles Production In development of ceramic tile samples, various raw materials mixes were processed sequentially using the process technology flow chart presented in Fig. 2. Figure 2. Process technology flow chart. The milled powder clay, quartz, feldspar and glass bottles were individually measured appropriately as indicated in Table 1 using a 0.001mg sensitivity weighing scale. The samples were sieved with 100 µm mesh and mixed to homogeneity. Subsequently, the mixed material (granulated powder mixture) was poured into a prepared mould, 5cm × 5cm size (Fig. 3) to form shaped test specimens and then uniaxially compacted using hydraulic press (Weber- Hydraulic, AC-8800 Vibrorg, Denmark. Type; p-16H, Capacity; 16T, S/N; 29580) under a pressure of 50 MPa, in accordance with guidelines in mould Pressed Ceramic Tiles - Specification (First Revision of IS 15622) ICS91.100.23. The pressed specimens were held overnight and then dried at 90 - 100°C for 48 hours in an oven. Dried specimens were fired in a laboratory type electric furnace (Nabertherm, more than heat 30- 3000°C) at the rate of 5°C/ min. The technological parameters values were measured after firing steps. The firing procedure used involves heating the sample at a temperature of 1170°C, then soaked for 3 hours and naturally cooled Correlia et al. (2004). The procedures were repeated for all the formulations (A- 55 The Journal of Engineering Research (TJER), Vol. 16, No. 1 (2019) 53-62 56 D). The produced samples of the ceramic tile specimens produced are shown in Fig. 4. 2.4 Determination of the Specimens’ Properties Some properties of the material mixes (moulded specimens) were tested for proper evaluation of their suitability. The properties include fired shrinkage, apparent porosity, bulk density, porosity and compressive strength, chemical composition and microstructural test. For the products to be in compliance with National and International Standards, these properties were evaluated using various national and international test procedures and standards as presented in Table 2. 2.4.1 Porosity of the Brick Sample Porosity of the brick sample was determined using ASTM JISD4418-1996 guidelines by soaking the bricks in a bath of water at 1000C for 8 hours. The mass of each of the samples before and after Figure 3a. The Mould. Figure 3b. Samples of ceramic tile specimens. Table 2. Various National and International test procedures and Standards used for evaluation of the samples. S/N Test procedures Standards 1 Specific gravity MS 474: Part 1: 2003 2 Compressive strain test method MS ISO 6310:2003, Part 4 3 Determination of modulus of rupture and breaking strength MS ISO (Part 6): 2006 (first revision) 4 Shear test procedure MS ISO 6312:2003, Part 6 5 Determination of thermal Conductivity ISO 7882: 1986 6 Porosity & Apparent porosity measurement JIS D 4418 – 1996 7 Determination of linear thermal expansion (Part 4): 2006 (first revision) 9 Determination of water absorption and bulk density. (Part 2): 2006 (first revision) DOC NO. CED 5(7888), Title: Pressed Ceramic Tiles – Specification (First Revision of IS 15622) ICS91.100.23. soaking was determined (in mg) and recorded. The porosity of the samples were then determined using equation 1. Porosity (p) 100 V 2M1M            (1) Where M1 is the mass (g) of brick before soaking, M2 is the mass (g) of brick after soaking water, ρ is the density of the liquid and V is the volume of sample (cm 3 ). 2.4.2 Apparent Porosity and Bulk Density of the Brick Samples The apparent porosity of each of the brick samples was also determined in accordance with JIS D 4418 – 1996. Brick samples (5 × 5 cm 2 ) dimension were used. The samples’ dried weight in air (Wsw) and the saturated (Wsa) of each sample were determined. The apparent porosity (Pa) and bulk density (ρb) of each brick was determined using the relationships in equation 2 and 3 respectively. Apparent porosity (Pa) 100 swWsaW daWsaW     (2) Bulk density (ρb) swWsaW daW   (3) 2.4.3 The Compressive Property The compressive property test was conducted on the brick samples using Testometeric Universal Testing Machine [TUF – C- 1000 KN (SI)] as specified by the MS ISO (part 6):2006 standard. Brick samples with diameter of 5 × 5 cm 2 were loaded gradually in compression until the brick failed to offer further resistance to deformation which was indicated by the bricks fracture. Various properties (stress, strain, extension and energy at different stages) of the samples were recorded from the display unit (monitor) attached to the machine. 2.4.4 Measurement of Fired Shrinkage The shrinkage properties of the bricks were determined by measuring both the green and fired dimensions of the 5 × 5 cm 2 brick samples, using Length Comparator with Digital Indicator in accordance with the guidelines in ASTM C227 / and as specified by the ISO 10545-2 standard. Both sides of the specimens were measured and the average linear shrinkage was calculated. The linear shrinkage of each side was calculated as a percentage of the original green dimension as expressed in equation 4. Linear Shrinkage (Ls) 100 gL fLgL    (4) where Lg and Lf are green and fired length of bricks respectively. 56 Z.U. Elakhame, Y.L. Shuaib-Babata, and I.O. Ambali 57 3. RESULTS AND DISCUSSION 3.1 Materials Chemical Composition The results of the chemical analysis in Table 3 show the major constituents of the clays, quartz and feldspar. 3.2 Porosity and Bulk Density The porosity and bulk density values of the various produced moulded ceramic tiles samples are as shown in Fig. 4 and 5 respectively. The specimens’ average porosity measurements ranged between 0.1 and 2.7%. It is shown in the results (Table 2) that 80% and the above constituents of the clay and feldspar were silica (SiO2) and Alumina (Al2O3). Clay possessed 59.2% silica and 21.25% alumina, while fledspar had 49.16% and 34.02% of silica and alumina respectively. Therefore, the clay and feldspar belong to Alumino-silicate group in line with the view of (Shuaib-Babata 2016; Abolarin et al. 2006; Hassan 1993; Encyclopedia Britannica (2018a; and Bastin 2018). Quartz also had silica as its major constituents with 99.96% value. Hobalt (2018) and Encyclopedia Britannica (2018b) affirmed that quartz primarily consists of silica. It is observed from Fig. 4 that the fraction of the volume of the voids over the surface of the specimens produced were very closed-cell foam. However, the results revealed that specimens 6 and 8 in formulation C had the lowest porosity values of 0.1%. This might be the result of reduction in the clay percentage in the composition of the specimens. Materials with low Table 3. The Chemical Compositions of all the raw solid minerals. Figure 4. Average porosity values of different moulded ceramic tiles samples with varying Compositions. Figure 5. Average bulk density values of different moulded ceramic tiles samples with varying composition. 0 0.5 1 1.5 2 2.5 3 1 2 3 4 5 6 7 8 P o ro si ty ( % ) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2 1 2 3 4 5 6 7 8 B u lk d e n si ty ( g /c m 3 ) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) S/N Parameters Level of Detection (wt%) Clay Quartz Feldspar 1 SiO2 59.200 99.96 49.16 2 TiO2 0.005 0.047 0.01 3 Al2O3 21.250 0.041 34.02 4 Fe2O3 15.700 0.006 0.74 5 CaO 1.920 0.100 2.87 6 MgO 0.880 0.007 0.08 7 Na2O 0.050 0.000 2.63 8 K2O 0.040 0.000 8.40 9 MnO 0.010 0.008 0.002 10 Moisture 0.002 0.001 0.005 57 The Journal of Engineering Research (TJER), Vol. 16, No. 1 (2019) 53-62 Figure 6. Average linear shrinkage values of different moulded ceramic tiles samples with varying Compositions. Figure 7. Apparent porosity values of different moulded ceramic tiles samples with varying Compositions. 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 1 2 3 4 5 6 7 8 Li n e a r s h ri in k a g e ( m m ) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) 0 20 40 60 80 100 120 1 2 3 4 5 6 7 8 A p p a re n t p o ro si ty ( % ) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) Figure 8. Stress – strain relationship in formulation A. 58 Z.U. Elakhame, Y.L. Shuaib-Babata, and I.O. Ambali porosity value are more preferred for production of tiles Elakheme et al. (2016). Generally, the average porosity values were within the recommended value of 0.1- 3.5% for tiles (National Research Council of Italy, 2017). The specimens’ average bulk densities were within 1.033 and 1.875 g/cm 3 (Fig. 5), which fall within the recommended standard bulk density range of 1.0 to 2.5 g/cm 3 for tiles (Hassan, 2011; National Research Council of Italy, 2017) and 1.7 –2.1g/cm3 for dense ceramic materials Hassan (2001). Sample 4 in formulation D had the lowest bulk density value of 1.033 g/cm 3 , while samples 5 & 6 in body formulation C recorded the highest value of 1.87 g/cm 3 . Materials with low density would be better for production of tile. 3.3 Fired Shrinkage and Apparent Porosity The samples’ linear shrinkage ranged between 0.08 and 0.40 mm (Fig. 6), which were within the accepted range of 0.02 and 0.80 mm (National Research Council of Italy, 2017). The samples’ linear shrinkage values at 1100 o C were significantly low. This is very advantageous for wall and floor tiles composition, which may be due to the presence of appreciable SiO2 in the composition. However, the magnitude of shrinkage increases with clay contents but the limit is reached for higher specific water contents Boivin et al. (2004). The samples’ calculated percentage apparent porosity ranged between 45.0 to 98.1%. These values were within the specified 30.0 to 60.0% values (National Research Council of Italy, 2017). Sample 8 in formulation A (80% and 20% quartz) had the lowest apparent porosity value of 45%, which is considered to be the best. This might be attributed to high proportion of SiO2 in the composition. High shrinkage resulted to reduced apparent porosity in the closure of internal pores. 3.4 Compressive Strength Test Figs. 8 to 11 show the stress-strain relation of the samples, which are better illustrated in Figs. 12 and 13 as an indicator for durability of the samples in service. The variations of calculated apparent porosity values in various samples of the composite are as presented in Fig. 7. Figure 9. Stress–strain relationship in formulation B. Figure 10. Stress–strain relationship in formulation C. 59 The Journal of Engineering Research (TJER), Vol. 16, No. 1 (2019) 53-62 Figure 11. Stress–strain relationship in formulation D. Figure 12. Average Compressive strength values of different moulded ceramic tiles samples with varying composition. Figure 13. Average energy at maximum stress by different moulded ceramic tiles samples with varying composition. Table 4. Summary of the sample’s properties compared with the available information on the properties of tiles. S/N Properties Tiles {CY + QZ & Dolomite} [National Research of Italy, 2017] New Formulation Lab. Tiles {CY + QZ + MG & Alumina} 1 Compressive strength (MPa) 5.000 - 20.800 1.0117 - 14.331 2 Bulk density (g/cm3) 1.0-2.5 1.2 - 1.8 3 Porosity measurement (%) 0.1-3.5 0.1 - 2.7 4 Apparent Porosity % 30 – 60 45 – 98 5 Shrinkage measurement 0.02-0.80 0.08 - 0.4 0 2 4 6 8 10 12 14 16 1 2 3 4 5 6 7 M a x im u m c o m p re ss iv e s tr e ss ( M P a ) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) 0 2 4 6 8 10 12 14 1 2 3 4 5 6 7 E n e rg y a t m a x im u m s tr e ss ( j) Various samples of the composites Clay+Quartz (A) Clay+Feldspar (B) Clay+Milled Glass ( C ) Clay+M.G+Q+F (D) 60 Z.U. Elakhame, Y.L. Shuaib-Babata, and I.O. Ambali Within the formulation A, B, C and D, sample 4, 2, 5 and 4 exhibited the highest compressive strength values of 6.98156 MPa, 14,33139 MPa, 11.45160 MPa and 8.83201 MPa respectively in each formulation group. These strength values were within the recommended range of 5.00 to 20.8 MPa for tiles Krivandin and Markiov (1980). However, other samples that had strength values within the recommended values include samples 1, 2, 4, 5 and 6 in formulation B, samples 1, 2, 3 and 4 in formulation B, and samples 2, 4 and 5 in formulation C (Fig. 12). From the obtained results, sample 2 in formulation B consisting of 80% clay and 20% feldspar exhibited the highest average compressive strength values (14,33139 MPa). This might be as a result of combination of high SiO2 with Al2O3 from both clay and feldspar. Samples 4, 2, 5 and 4 respectively in formulation A, B, C and D also had energy at maximum stress of 4.74391 J, 11.77584 J, 9.53256 J and 7.5682 J respectively, in each formulation group. Generally, the energy values exhibited by the samples ranged between 0.02818 and 11.77584 J. The majority of these energy values were considered to be adequate for sustainability of the tiles in service. To determine the stability of the samples, it is essential to compare the properties exhibited by the samples with that of available information on the properties of ceramics tiles as presented in Table 4. Thorough critical study of the data in Table 3 shows that various properties exhibited by sample 4 (formulation A), sample 2 (formulation B), sample 5 (formulation C) and sample 4 (formulation D) met the required standards for tiles. Therefore, the new formulation for production of ceramics tiles using locally available raw materials (clay, quartz, feldspar and milled bottles) proved suitable and adequate for local production of composite ceramic tiles in terms of strength and other properties. This will assist to address the nation’s economic problems and help towards job creation. 4. CONCLUSION From this study, the following conclusions are drawn: 1. The clay and feldspar used in this study were found to belong to alumino-silicate group. 2. Suitable combinations of Nigerian natural resources and wastes such clay, feldspar, quartz and milled glasses were found suitable for the production of standard ceramic tiles. The suitable proportions of the materials in production of the tiles: 60: 40%, 80:20%, 50:50% and 60:5:5:30% of clay and quartz, clay and feldspar, clay, quartz and feldspar, quartz, feldspar and milled glasses respectively. 3. Clay, quartz, feldspar and milled glasses were characterized to ascertain for their potentials for ceramic tiles, refractory and others ceramics applications. The results obtained showed that they meet the criteria for use as refractory/ceramic raw materials in the entire characteristic investigated via chemical composition, fired shrinkage, porosity, apparent porosity, bulk density and compressive strength. The clay can be used as a fired refractory, while quartz, feldspar and milled bottles could be used as a source of silica and alumina for ceramic products. 4. 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