Ceramic Tile Formulations from Industrial Waste

02•10 APRIL VOL. 59 INTERCERAM 59 (2010) No. 2 pp. 79–166

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Ceramic Bricks Filling – Energy Saving

J.A. Junkes1, M.A. Carvalho2, A.M. Segadães3, D. Hotza1 Building Materials

Effect of Bi2O3 on Cordierite Formation in Cordierite Based Bodies

Ceramic Tile Formulations from Industrial Waste TILE & BRICK

The Use of Residues in the Manufacture of Ceramic Tile Bodies Hot-Pressed Gres Porcellanato Body Effect of Calcite on the Brick Body Closing Glossiness and Slipperiness of Polished Porcelain Stoneware Tiles Effect of Diaspore Addition on Microwave-Assisted Sintering of Floor Tile

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The authors The main author, Janaína Accordi Junkes, received a MSc in Materials Engineering from the Federal University of Santa Catarina, Brazil. She is currently earning her Doctorate in Materials Science and Engineering at the same university. As part of her research, she has also spent time at the University of Aveiro in Portugal. Ms. Junkes is one of 20 young scientists from around the world, who won the “Green Talents 2010 – International Forum for High Potentials in Sustainable Development” Competition of the German Federal Ministry of Education and Research (BMBF) for her work on reusing mineral waste for tile manufacturing. In her research activities, she is focusing on waste treatment, zeolites, ceramic materials, ceramic processing, and waste management. E-mail: [email protected] The corresponding author, Dachamir Hotza, earned his PhD (Dr.-Ing.) from the Technical University of HamburgHarburg (Germany). During his postdoctoral studies he did research at the University of Erlangen (Germany), OMTRI (Japan), and University of Queensland (Australia). He is currently Associate Professor at the Department of Chemical Engineering and the Graduate Program on Materials Science and Engineering at UFSC, Brazil. Prof. Hotza’s research interests include recycling of solid wastes, ceramic processing, nanotechnology, and rheology. E-Mail: [email protected]

Maria Arlete Carvalho earned her MSc in Ceramic and Glass Engineering from the University of Aveiro, Portugal. She is currently working on her PhD in the Materials Science and Engineering Department of the same university. Her main research interests are: development of new materials, study and optimization of processes in the area of ceramic materials/construction ceramic materials, as well as the behaviour of magnesium phosphates. E-mail: [email protected]

Ana Maria Segadães earned her PhD in Chemical Engineering from Sheffield University, UK. After this, she worked as postdoctoral researcher at the University of California in Santa Barbara, USA, and in Brazil. At present she is Associate Professor at the Aveiro University, Por tugal. The research areas of Prof. Segadães are: phase diagrams and ceramic processing in general, refractory castables, hydration behaviour of calcium aluminates and magnesium phosphates, structural porous ceramics with engineered microstructure, combustion synthesis of ceramic oxide powders, design of experiments, reuse and recycling of industrial wastes and sub-products. E-mail: [email protected]

Abstract In recent years scientific issues related to environmental preservation have acquired great importance and a major challenge to be met is the recycling of materials discarded by various productive sectors. Due to the damage caused to the environment by technological development through the disposal of waste, this study seeks to evaluate the possibility of using industrial waste as alternative raw materials in the manufacture of ceramic tiles. Different industrial wastes that are classified as non-hazardous were selected: sludge from the crushing process of gneiss, sludge from the cutting and polishing process of varvite, sludge from the process of filtration-clarification of potable water and a clay also classified as waste. As it was generated, all waste was dried and disaggregated in ball mills, and characterized by X-ray fluorescence, Xray diffraction, differential thermal and gravimetric analysis, optical dilatometry, and particle size distribution. The applicability of these wastes in the manufacture of ceramic tiles was guided by the phase dia-

gram of the system S–K–A, and four formulations were established. For initial testing, these formulations were mixed and pressed into pellets, and sintered at 900 °C, 950 °C, 1000 C, 1050 °C, 1100 °C, and 1150 °C. The plasticity formulations were evaluated by the Casagrande method with good results. Moreover, based on those preliminary results and after optimization of the processing conditions, the extrusion technique was used for the shaping process. The extruded samples were fired at 1100 °C and 1150 °C for 40 min and characterized by X-ray diffraction, differential thermal and gravimetric analysis, optical dilatometry, linear shrinkage, water absorption, and flexural strength. The crystalline phases identified were associated with the sintering conditions (temperature, time, atmosphere), as well the intrinsic characteristics of raw materials such as chemical composition, particle size and homogeneity. The wastes proved to be good alternative raw materials and the corresponding formulations were shown to be viable in the manufacture of ceramic tiles.

Keywords waste, tile, ceramic formulation, phase diagrams Interceram 60 (2011) [1]

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Group of Ceramic and Glass Materials (CERMAT), Departments of Mechanical Engineering (EMC) and Chemical Engineering (ENQ),, Federal University of Santa Catarina (UFSC), 88040-900 Florianópolis, SC, Brazil. Contact: [email protected] Polytechnic Institute of Viana do Castelo (ESTG-UIDM), 4900-348 Viana do Castelo, Portugal Department of Ceramics and Glass Engineering (CICECO), University of Aveiro (UA), 3810-193 Aveiro, Portugal

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1 Int The c of com manu fore, t dition recove Solid indus water porta ate wa gener It is o simila raw m not o manu The fa advan highly due to portu ularly [3]. It diagra ramic ing g proce A grea raw m inert) (SiO2) nor a presen of th Cr2O3 tant r low te (MgO have a The p concis the eq tion, t may p propo ing, i. tering line p agram ed fro rium basis behav ice or comp the ph tem m Altho condi usuall

l Engis, she sity of resent y, Por phase actory minates neered sign of ts.

ed. For ellets, 150 °C. method nd afhnique red at action, linear phasature, terials wastes ng fortiles.

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ic and rtugal. als Sciersity. w maarea of as well

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1 Introduction The ceramic industry covers a diverse range of compounds, and several products can be manufactured by different methods. Therefore, this industry presents favourable conditions for the implementation of waste recovery systems. Solid wastes are generated as by-products of industrial processes or as sludge from wastewater treatment plants. It is therefore important to know the operations that generate waste, as well as the factors that affect its generation in manufacturing processes [1]. It is often overlooked that some wastes are similar in composition when compared to raw materials, containing materials that are not only compatible, but beneficial to the manufacture of ceramics [2]. The fabrication of products from waste is an advantage that may give the manufacturer a highly competitive position in the market due to economic issues involved and the opportunity of marketing this principle particularly with regard to the ecological aspect [3]. It is in this context that the use of phase diagrams becomes a useful tool to guide ceramic production and also to assist in making good choices of composition and processing parameters. A great deal of solid wastes, as well as natural raw materials (whether plastic, fluxing, or inert) contain, as major components, silica (SiO2), alumina (Al2O3) and lime (CaO). Minor amounts of other components may be present, which will mostly affect the colour of the fired product (Fe2O3, MnO, TiO2, Cr2O3) but should not play such an important role during ceramic processing in air at low temperatures. Other minor components (MgO, K2O, Na2O) will act as fluxes and may have a strong effect during sintering [4]. The phase diagrams provide a clear and concise method of graph representation of the equilibrium state for a given composition, temperature and pressure [5], and this may provide a valuable estimate of the phase proportion present during and after sintering, i.e. the presence of liquid phase at sintering temperature and the resulting crystalline phases [6]. Stable phase equilibrium diagrams represent phases that may be expected from reactions occurring under equilibrium conditions and, therefore, provide a basis for making predictions of the material behaviour under various conditions of service or processing. Not all reactions reach complete equilibrium, and consequently, the phases which are present in a given system may not be the equilibrium phases [7]. Although in normal industrial operating conditions thermodynamic equilibrium is usually not reached, the equilibrium phase


diagram of the relevant system can still be used to foresee the reactions’ tendency to completion and be of great assistance for making appropriate choices of compositions and processing parameters [6]. Although it is a possibility and a priority to reduce the amount of waste during production and even post-consumer use, waste will always be generated. Sustainable development requires a reduction in consumption of natural raw materials that are not renewable. The closure of the production cycle, generating new products from recycled waste, is an irreplaceable alternative. The use of wastes from the beneficiation of ornamental rocks has been investigated, usually by the addition of up to 50 mass-% of waste into clayish products [8–11]. The wastes may be used to replace conventional flux materials, with the advantage of controlling the plasticity and shrinkage of the ceramic body without producing any negative effect on the product properties, and allowing sintering at low temperatures, thus resulting in energy conservation. This work aims to formulate new ceramic tiles from mineral wastes, based on phase diagrams, allowing the withdrawal of those residues from the environment and giving them a nobler destination. U1_U4_IC_2_10.indd 2

2 Experimental Mineral wastes with the potential of being reclaimed through their use as alternative raw materials in the ceramic industry were selected from Santa Catarina state, Brazil. The selected wastes were: sludge from the crushing process of gneiss, sludge from the cutting and polishing process of varvite, sludge from the process of filtration/clarification of potable water, and an iron-containing residual clay.

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A relevant ternary system was chosen to guide the formulation of products. The mixtures were prepared with the as-received raw materials, according to the predetermined amounts. The formulations were homogenized with a blender (Gelenski, LIG-05) and molded in an extruder with a matrix adjusted for producing cylindrical specimens. After extrusion, the specimens were airdried at room temperature and sintered at 1100 °C and 1150 °C with a heating rate of 5 °C/min for 40 min. For sintering, a laboratory oven (Termolab) with a maximum working temperature of 1700 °C was used. The chemical composition of the wastes was determined by X-ray fluorescence (Philips, PW 2400). The mixtures were analyzed by X-ray diffraction (Philips, Xpert), particle size distribution (laser diffractometer CILAS, 1064L), differential thermal and thermogravimetric analysis (Netzsch, 409 EP). The Casagrande method was applied to evaluate the plasticity of mixtures, and tests of linear shrinkage, water absorption and three-point flexural strength were accomplished in a universal testing machine (Shimadzu AG-25TA). The microstructural analysis of fracture surfaces was performed by scanning electron microscopy (Shimadzu, SSX-550). The Glass Industry in the EU Today – a Survey



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3 Results and discussion The chemical compositions of the four wastes investigated in this work are shown in Table 1, as well as the average particle sizes as determined by laser diffraction. The average particle size (d50) is between 4 and 13 μm, which may favour obtaining good mixing and suitable packaging in the forming step.

Table 1 • Chemical composition and average particle size Oxides

Clay / mass-%

PWS / mass-%

Gneiss / mass-%

Varvite / mass-%

SiO2

63.01

53.30

59.22

74.32

Al2O3

19.55

22.10

16.75

8.79

Na2O

0.05

0.24

4.48

3.12

K2O

2.83

2.11

4.31

1.48

CaO

0.04

0.12

5.98

2.68

MgO

0.77

1.20

1.63

1.74

Fe2O3

6.51

7.02

4.56

2.43

MnO

0.02

0.09

0.14

0.16

TiO2

0.91

0.83

0.43

0.51

P2O5

0.07

0.24

0.75

0.18

Loss on fire

6.30

12.76

1.74

4.59

Particle size / µm

5.30

4.37

13.37

7.87

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Building Materials Effect of Bi2O3 on Cordierite Formation in Cordierite Based Bodies

TILE & BRICK The Use of Residues in the Manufacture of Ceramic Tile Bodies Hot-Pressed Gres Porcellanato Body Effect of Calcite on the Brick Body Closing Glossiness and Slipperiness of Polished Porcelain Stoneware Tiles Effect of Diaspore Addition on Microwave-Assisted Sintering of Floor Tile


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The wastes are composed predominantly of silica and alumina, also containing high percentages of iron oxide (III) and potassium oxide. The waste with the highest loss on firing (~13 %) was potable water station (PWS) sludge due to constitutional water and organic matter. From the chemical analysis data, one point for each waste was traced within the chosen phase diagram (SiO2–Al2O3–K2O). The effect of oxide fluxes on the system Al2O3–SiO2 was discussed in terms of the junction of the components CaO + MgO + K2O + Na2O. All formulations set forth in this study are positioned within the mullite field, as shown in Fig. 1. According to the diagram, four formulations were chosen. The mass-% of each waste in the formulations is presented in Table 2. To identify the mineralogical phases X-ray diffraction was used. Figure 2 shows the X-ray diffraction patterns of the formulations F1, F2, F3 and F4 sintered at 1100 °C and 1150 °C for 40 min. The variations with the increase of sintering temperature may

3

Fig. 3 •

4

Fig. 1 • SiO2–Al2O3–K2O phase diagram including the compositions of waste raw materials and formulations

2

Fig. 4 •

be o diffra F1 sh anort (KAlS mullit as a r ing ca presen of qu (Fe2O

Fig. 2 • X-ray diffraction of the samples sintered at 1100 °C and 1150 °C: (a) F1, (b) F2, (c) F3, (d) F4


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one in the K2O). ystem of the MgO + rth in mul-

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mulaeach ed in

X-ray ws the mula100 °C s with e may

Fig. 3 • DTA/TG curves: (a) F1, (b) F2, (c) F3, (d) F4

Fig. 5 • Linear shrinkage (a) and water absorption (b) of samples sintered at 1100 °C and 1150 °C

4 Table 2 • Mixture formulations

Fig. 4 • Liquid limit plot of according to Casagrande’s method: (a) F1, (b) F2, (c) F3, (d) F4

be observed with the superposition of diffraction patterns. F1 showed peaks of albite (NaAlSi2O8), anorthite (CaAl2Si3O8), orthoclase (KAlSi3O8) and microcline (KAlSi3O8). The mullite (3Al2O3·2SiO2) peaks were formed as a result of kaolinite transformation during calcination of clay and the PWS sludge present in the formulation. At 1150 °C peaks of quartz, albite, mullite, and hematite (Fe2O3) are evident.


Peaks of mullite and hematite were found as well as peaks of quartz and anorthite at 1100 °C and 1150 °C in F2. F3 presents peaks of quartz, albite and anorthite. Magnesium silicate (enstatite, Mg2(Si2O6)) was also identified. This silicate was possibly formed from the decomposition of clinochlore ((Mg,Fe)5Al(Si3Al)O10(OH)8) originally present in varvite. In the diffractogram of F4 at 1100 °C peaks of quartz, anorthite and mullite were ob-

Formulation

Waste / mass-%

F1

F2

F3

F4

Clay

40

20

20

30

PWS

10

65

10

20

Gneiss

45

10

5

10

Varvite

5

5

65

40

served, and at 1150 °C peaks of quartz, mullite, albite, mayenite (Ca12Al14O33) and hematite were observed. The diffractograms of the four formulations presented mullite peaks in accordance with the provided from phase diagram, but due to the amount of components present in these four wastes, this resulted in the presence of several other phases. The thermal behaviour of the formulations was analyzed through DTA/TG curves shown in Fig. 3. In the DTA curve of F1 the release of free water at 110 °C and a loss of organic matter around 280–500 °C may be observed. The endothermic peak at 570 °C corresponds to the release of constitution water from clays, and a slight exothermic peak around 982 °C (without mass loss) corresponds to the onset of mullite formation (as identified by XRD). The corre-

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Fig. 6 • Visual aspect of samples sintered at 1100 °C and 1150 °C

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Fig. 7 • Flexural strength of samples sintered at 1100 °C and 1150 °C

sponding mass losses are visible in the TG curve, with total mass loss of 10 %. In F2 the same peaks found in F1 were identified: water loss at 110 °C, release of organic matter around 250–520 °C, and constitution water from clays at 570 °C. However, due to the 65 mass-% PWS sludge content in this composition, F2 showed an exothermic peak around 610 °C due to the sulphate decomposition, which is introduced in the potable water station for particle flocculation. The total mass loss of this formulation was 16 %. The first three peaks of F3 were also identified in F1 and F2. Besides these peaks, an endothermic peak around 820 °C was found, which is probably related to the carbonate decomposition (dolomite) present in varvite; a component that corresponds to 65 mass-% in this mixture. It is also possible to observe a slight exothermic peak around 980 °C (without mass loss) due to the onset of mullite formation as identified by XRD. The test result obtained from F4 is similar to that obtained from F3. However, the peak corresponding to the carbonate decomposition around 800 °C is less pronounced due to a decrease of varvite content from 65 to 40 mass-%, which thereby reduces the amount of carbonate present in the formulation. In spite of the mullite detected in the corresponding XRD pat-


Fig. 8 • Fracture surface micrographs of samples sintered at 1100 °C and 1150 °C

tern, the formation peak of mullite is not visible in the thermal analysis. The distinct thermal behaviour was probably due to different heat cycle employed. The extrusion was used because it is a lowcost forming technique with a high production output. However, this fabrication alternative requires that the formulations exhibit plasticity. The Atterberg method was used to determine the moisture content corresponding to plastic and liquid limits. The procedure for determining the liquid content was performed for several amounts of water content using Casagrande’s method, as shown in Fig. 4. The plastic limit was measured using the rolls

method. The plasticity index (PI) was then calculated as the difference between both limits. PI determines the plasticity nature of the sample, thus, as high is PI, more plastic is the raw material. According to Caputo [12], except for F3, which presented PI=14.4 %, and corresponds to a moderately plastic material, all formulations can be classified as highly plastic since their PI is higher than 15 %. Samples sintered at 1100 °C and 1150 °C were tested for shrinkage and water absorption, as shown in Fig. 5. After sintering at 1150 °C, F1, F3, and F4 showed apparent bubbles and distortion of the specimen. F1 presented 4.6 % shrinkage and water ab-

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sorpti 1100 ° with a to 0.5 aroun 0.80 % sinter vere d ed in t at 110 tion t a sligh the sa and 1 pores The sa at 115 rosity lower The w 10 %, specif tion 1100 ° ceram ard N Figure mens ing m F4 sin The s influe in Fig at 115 and i phase streng Samp streng high t visual ture fo The f was in within the m excep would tiles, produ The m formu

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sorption around 9 % when sintered at 1100 °C; at 1150 °C the shrinkage was 6 % with a marked decrease in water absorption to 0.56 %. Samples F2 showed shrinkage around 14 % and water absorption around 0.80 %, both for 1100 °C and 1150 °C. F3 sintered at higher temperature presented severe distortion and pores, which was reflected in the results of linear shrinkage (10.41 % at 1100 °C and 2.51 % at 1150 °C). In relation to water absorption, the results showed a slight difference (less than 1 %) between the samples sintered at 1100 °C (0.46 %) and 1150 °C (1.27 %), despite the number of pores introduced at higher temperature. The same occurred with F4 samples sintered at 1150 °C, although the distortion and porosity developed with the temperature was lower in this case. The water absorption of all samples is below 10 %, which is compatible with the range specified for ceramic tiles. With the exception of F1, all formulations sintered at 1100 °C were within the values expected for ceramic tiles, according to Brazilian standard NBR 13818. Figure 6 shows the visual aspect of the specimens after sintering. Distortion and swelling may be observed in samples F1, F3 and F4 sintered at 1150 °C. The sintering temperature had a significant influence on the flexural strength, as shown in Fig. 7. The thermal treatment performed at 1150 °C induced the formation of cracks and internal porosity due to the liquid phase, causing a decrease in mechanical strength in samples F3 and F4. Samples F1 and F2 presented higher flexural strength at 1150 °C than 1100 °C, but the high temperature affected all samples in the visual aspect, which is a very important feature for ceramic tiles. The flexural strength of all samples tested was in the range of 21–58 MPa, which is within the range required by ISO 13006 for the manufacture of ceramic tiles. With the exception of formulation F1, the samples would even be classified as porcelainized tiles, corresponding to a higher quality product. The morphological characterization of the formulations was performed by scanning

electron microscopy on fracture surfaces of samples subjected to mechanical strength test. Figure 8 shows the micrographs of samples sintered at 1100 °C and 1150 °C. F1 sintered at 1100 °C presented less porosity and irregularity when compared to the samples sintered at 1150 °C. F2 showed a high linear shrinkage in the samples, resulting in the formation of cracks. F3 was well consolidated at 1100 °C but when sintered at 1150 °C it developed a large amount of pores of different sizes that were visible even to the naked eye. F4, sintered at 1100 °C, showed a small amount of micropores, but was as dense as the sample F3 sintered at 1100 °C, when sintered at 1150 °C, however, it developed a large amount of porosity, which affected its mechanical properties and visual aspect.

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The mechanical strength of the formulated samples is within the range of 21–58 MPa, which complies with requirements of ISO 13006. The possible applications of such ceramic tiles may be on floors and walls, indoors and outdoors, for commercial and residential installations. The Glass Industry in the EU Today – a Survey


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4 Conclusions The results confirmed the possibility of valorisation and recycling of mineral wastes from the state of Santa Catarina, Brazil, as sources of raw materials for the ceramic tile industry. Thus, these industrial wastes may be used as products with higher added value with positive effects with respect to environmental and economical issues. The four wastes studied are an attractive alternative and renewable source of ceramic raw materials. Glazing would not be required for these tiles, making the process even more affordable, since these products would be classified as natural products, where the colour of the waste determines the colour of the finished product. The phase diagram was used successfully to guide the formulations and to help choosing the process parameters. In all cases, it provided a basis for making predictions of material behaviour under several conditions of service or processing. Forming by extrusion is feasible for the processing of these materials because the amount of plasticity is large enough; the plasticity index being higher than 14, with no need for additives. The shrinkage, water absorption, and mechanical strength tests indicated that the best firing cycle to be used with those alternative raw materials is at 1100 °C for 40 min.


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Acknowledgment The authors thank CNPq-Brazil for the financial support.

References [1] Teixeira, S.R, Souza, S.A., Souza, N.R., Job, A.E., Gomes, H.M., Heitzmann Neto, J.F.: Caracterização de resíduos de estações de tratamento de água (ETA) e de esgoto (ETE) e o estudo da viabilidade de seu uso pela indústria ceramic. XXVIII Congresso Interamericano de Ingeniería Sanitaria y Ambiental, Cancun (Mexico), 27–31 October 2002 [2] Santos, P.S.: Ciência e Tecnologia de Argilas, volume 1. Edgard Blücher, São Paulo (1997) [3] Modesto, C., Bristot, V., Menegali, G., De Brida, M., Mazzucco, M., Mazona, A., Borba, G., Virtuoso, J., Gastaldon, M., Novaes de Oliveira, A.P.: Obtenção e Caracterização de Materiais Cerâmicos a partir de Resíduos Sólidos Industriais. Cerâmica Industrial 8 (2003) [4] 14–18 [4] Segadães, A.M.: Use of the diagrams to guide ceramic production from wastes. Advances in Applied Ceramics 105 (2006) 46–54 [5] Kingery, W.D., Bowen, H.K., Uhlmann, D.R.: Introduction to Ceramics, 2nd edition. John Wiley & Sons, New York (1976) [6] Raupp-Pereira, F., Hotza, D., Segadães, A.M., Labrincha, J.A.: Ceramic formulations prepared with industrial wastes and natural sub-products. Ceramics International 32 (2006) 173–179 [7] Bergeron, C.G., Risbud, S.H.: Introduction to Phase Equilibria in Ceramics. The American Ceramic Society, Westerville, Ohio (1984) [8] Acchar, W., Ramalho, G., Fonseca, Y.A., Hotza, D., Segadães, A.M.: Using granite rejects to aid densification and improve mechanical properties of alumina bodies. Journal of Materials Science 40 (2005) 3905–3909 [9] Acchar, W., Vieira, F.A., Hotza, D.: Effect of marble and granite sludge in clay materials. Materials Science and Engineering A 419 (2006) 306–309 [10] Acchar, W., Vieira, F.A., Segadães, A.M.: Using ornamental stone cutting rejects as raw materials for red clay ceramic products: Properties and microstructure development. Materials Science and Engineering A 435–436 (2006) 606–610 [11] Segadães, A.M., Carvalho, M.A., Acchar, W.: Using marble and granite rejects to enhance the processing of clay products. Applied Clay Science 30 (2005) 42–52 [12] Caputo, H.P.: Mecânica dos Solos e suas Aplicações, volume 1, 6th edition. LTC, Rio de Janeiro (1998) Received: 18.11.2010

150 °C bsorping at parent en. F1 r ab-


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Ceramic Tile Formulations from Industrial Waste

Ceramic Tile Formulations from Industrial Waste

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