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Development of glass-ceramics from boron containing waste and meat bone ash combinations with addition of waste glass
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CERAMICS INTERNATIONAL
Ceramics International 40 (2014) 6045–6051 www.elsevier.com/locate/ceramint
Development of glass-ceramics from boron containing waste and meat bone ash combinations with addition of waste glass B. Ciceka,e,n, A. Tuccib, E. Bernardoc, J. Willd, A.R. Boccaccinid a Eczacıbaşı Building Products Co. VitrA Innovation Center, Turkey Department of Biomedical Science and Neuromotor Sciences, University of Bologna, Italy c Department of Industrial Engineering, University of Padova, Italy d Department of Materials Science and Engineering, University of Erlangen-Nuremberg, Germany e Centro Ceramico Bologna, University of Bologna, Italy b
Received 24 September 2013; received in revised form 11 November 2013; accepted 12 November 2013 Available online 20 November 2013
Abstract Glass-ceramic materials represent a great resource for environmental cleanup, because they can stabilize pollutants by vitrification and, at the same time, they may present remarkable mechanical and functional properties enabling novel applications. In this paper, different mixes of three different industrial wastes, namely boron waste (BW), meat bone and meal ash (MBM) and recycled soda lime silica glass (SLG) were prepared by considering the combined effects of thermal cycle requirement, particle sizes of the selected wastes and amount (content) of boron waste. Glass-ceramics were prepared from selected waste mixtures and the physical and mechanical properties of the obtained glass-ceramics were measured. The results underline that boron containing waste-derived glass-ceramics are attractive for applications as gas concrete blocks or as an additive in new generation insulation ceramics. & 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved. Keywords: Glass-ceramics; Borates; Waste recycling; Recycled glass; Building materials
1. Introduction Glass-ceramic materials feature a great potential for environmental cleanup, since they may combine waste stabilization and valorization [1,2]. The stabilization of pollutants is provided by vitrification, i.e. the formation of waste-derived glasses with significant durability, whereas valorization process comes from the controlled crystallization, leading to remarkable mechanical and functional properties of glass-ceramics [3,4]. Glass-ceramics derived from glasses obtained from a variety of wastes, e.g. metallurgical slags [5,6], residues from urban incinerations [7–9], coal ash from power stations [10], or mixtures of them, have been widely reported in the literature [1–4]. The high costs and energy consumption associated to the typical vitrification/ceramization process, however, still constitute an open issue. A possible solution, to be considered n Corresponding author. Eczacıbaşı Building Products Co. VitrA Innovation Center, Bozuyuk/Bilecik, Turkey. Tel.: þ 90 22 83140400; fax: þ90 22 83140412. E-mail address: [email protected] (B. Cicek).
especially for not particularly toxic wastes, comes from a substantial revision of the concept of glass-ceramics, based on direct sintering of inorganic waste, i.e. on a process resembling that of traditional ceramics. With a proper selection of the starting waste, a significant amount of liquid phase may form upon firing and later convert into a glass [11]. This glass may incorporate crystals from unreacted starting materials, as well as newly formed crystals [1,12]. In this paper we referred to combinations of three different industrial wastes, chosen to generate compositions belonging to the B2O3–P2O5–SiO2 (boro-phospho-silicate) ternary system, known to yield interesting glass and glass-ceramics for different functional applications (e.g. dielectrics) [13–15]. The durability of glasses of this system is quite poor, [14] but it may be substantially improved after crystallization by applying different heating rates [16]. The considered industrial wastes consisted of boron waste (BW), meat bone and meal ash (MBM) and recycled soda lime silica glass (SLG). Boron waste (also known as borate waste/boron containing waste), the source of which is essentially the extractive activity
0272-8842/$ - see front matter & 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved. http://dx.doi.org/10.1016/j.ceramint.2013.11.054
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(concentrator waste), has a rather broad phase composition [12]. Even if many studies underline that boron wastes can be used as additives in cement, [17] brick [18] and in the ceramic [19] production, to the authors' knowledge no industrial process, allowing an efficient use of large amounts of boron wastes, is available. The barrier in front of industrial utilization might be the operational difficulties. B-containing wastes have been already proposed to prepare glass ceramics [20–22]. Meat bone and meal ash (MBM), phosphate containing waste, are obtained by crushing bones and meats coming from slaughterhouses, that have no EU legislative approved hazardous compounds, such as brain, spinal cord or diseased animal waste (safe animal waste) and processing them in compliance with the regulatory codes [23,24]. MBM ash is obtained after heat processing the MBM wastes at 800–900 1C and removing all the organic substances, such as proteins. Usually, 100– 320 kg of MBM ash is obtained from a ton of MBM [25]. In European Union countries, especially in England and France, there are high-capacity MBM incineration plants. In France, the obtained MBM is burned together with coal at the rate of 45% to have clinker and the rest (1040 ktons) is reserved for future processes, still to be explored. [25] Soda lime silica glass (SLG) waste is one of the most important waste materials considering its production amount [27]. SLG is collected from windowpanes, bottles (containers), and glass products through various industries (glass packaging and other waste glass residues from municipal, commercial or industrial sources, mixed municipal solid waste and bulky waste etc.). In 2009, 11.5 million tons of packaging glass waste were collected from 27 E.U. countries, including Norway, Switzerland and Turkey. The packaging glass recycle ratio is 65% in EU countries [26] Many investigations have been carried out on the re-use possibilities of waste glasses, especially when glasses are colored and, therefore, hard to separate. Such investigations have generally been focused on utilizing glass residues in
glasses, [28] ceramics, [19,29,30] glass-ceramics, [31] and cements [22]. All these technologies are very attractive, but still need to be extended and further optimization studies are required. The present study aims at evidencing the feasibility of producing glass-ceramics by a combination of the mentioned wastes, applying low cost direct sintering treatments, in turn featuring high heating rates and relatively low maximum temperatures, with a specific attention to the stabilization of the toxic components such as high amount of Boron, possibly embedded in the starting materials, at the lowest possible energy consumption.
2. Experimental procedure 2.1. Materials and processing A colemanite enrichment tailing waste, from Eti Bor Bigadiç deposit (open pit), located in the Marmara region in Turkey, was used as boron waste (BW). The MBM ash was obtained from the Glanford Power Station (Scunthorpe, UK). SLG, provided by SASIL Life (Biella, Italy), was derived from municipal recycling with an off white color. The chemical composition of these wastes, determined with inductively coupled plasma optical emission spectroscopy (ICP-OES model 3200 XL Perkin Elmer, USA), is reported Table 1. The phase composition of the starting material and of the studied mixtures, after the thermal treatments, was determined by X-ray powder diffraction analysis (Philips PW3830, NL); phase identification was achieved by means of the Match! program package (Crystal Impact GbR, Bonn, Germany), supported by data from PDF-2 database (ICDD-International Centre for Diffraction Data, Newtown Square, PA). The thermal characterization of the starting materials was performed with the
Table 1 Chemical and mineralogical composition of used waste materials. BW Chemical composition, in oxides (wt%) 16.1 SiO2 0.2 Na2O K2O 0.5 MgO 6.9 CaO 26.4 SrO 1.2 Al2O3 0.9 Fe2O3 0.1 SO3 P2O5 B2O3 19.7 L.O.I. 28.0
MBM
SLG
2.3 8.7 3.5 1.3 46.4
71.6 13.5 0.4 3.9 9.0
0.2
1.0 0.1
3.6 34.0
Phase composition Calcite Colemanite Olshanskyte Ca Borate Hydrate
Hydroxyapatite Tricalcium phosphate
Amorphous phase
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Table 2 Details of the adopted combinations of formulation and heating rates. Mix
Sample
Heating rate 1C/min
Tmax/Holding time
Cooling
A
AF AH AS
16.5 16.5 2.6
950 1C/1 min 950 1C/1 h 950 1C/3 h
Fast, 1 h Fast, 1 h Slow, natural cooling
B
BF BH BS
16.5 16.5 2.6
950 1C/1 min 950 1C/1 h 950 1C/3 h
Fast, 1 h Fast, 1 h Slow, natural cooling
use of a heating microscopy (Expert System Solutions-Heating microscope HSM, IT). Two different mixtures were prepared. The first one, labeled A, contained 30 wt% of MBM, 30 wt% of BW and 40 wt% of SLG. Due to the presence, in BW, of crystalline phases, such as calcite (CaCO3) and colemanite (CaO 3B2O3 5H2), that released gases during the following heating step, the BW material was calcined at 500 1C. The calcined BW and MBM ash were milled to particle size o 200 mm. SLG was milled to particle size o 150 mm (Retcsh PM 100, Germany), as measured with a laser granulometer. Compared to the annual production amounts and re-use capacities of the selected wastes, BW is the most abundant one. For this reason, in the second studied composition, labeled “B”, always respecting the glass-ceramic ternary system, the amount of BW was increased up to its highest possible limit. As a result, B samples contained 40 wt% of BW and 30 wt% of MBM ash and SLG. It is known that colemanite (CaO 3B2O3 5H2O), present in the used BW, decomposes with the release of five molecules of H2O between 400 and 500 1C, by transforming into a fine particulate material, less than o 200 mm in size [35]. The temperature of onset of dehydration for colemanite is 262 1C and the first water molecule is lost at 327 1C, which coincides approximately with the onset of decrepitating. The last crystal water loss takes place at 412 1C [36]. Several studies underline that the calcination step of colemanite has an effect similar to a milling process [36]. With the aim to set up a production system for glass-ceramics, characterized by low energy consumption, the calcination step of the BW waste, used in B samples, was substituted by milling into finer particle size (o 80 mm). Sintering tests were performed on compacted powder specimens, uniaxially pressed in form of discs of 10 mm diameter and 4.5 mm in height, under a load of 50 kN. Specimens of both mixtures were sintered at 950 1C by using different heating rates. A fast sintering process was used, characterized by a heating rate of 16.5 1C/min up to the maximum heating temperature of 950 1C. The sintered samples are labeled “F”. The samples fired with the same heating cycle, but with 1 h of holding time at 950 1C, are labeled “H”. A rather rapid cooling from the sintering temperature was adopted for both sintering schedules, e.g. it took 1 h to reach room temperature. A slow sintering process was also used for comparison purposes. The heating rate was 2.5 1C/min up to the maximum
temperature of 950 1C, with 3 h of holding time followed by natural cooling. The samples sintered according to this schedule are labeled “S”. The details of the different sintering treatments are summarized in Table 2. 2.2. Mechanical and microstructural characterization The bulk density of fired materials was determined by their weight and volume determination. The mechanical strength of the different sintered samples was measured by the Brazilian test method [37,38]. This method is also known as “diametral compression” and “indirect (splitting) tensile test”, and it is used as an indirect experimental method to measure the tensile strength of materials [39]. One reason to select the Brazilian test method is that it employs samples of simple form (disc shape) as opposed to the flexural strength text which requires prismatic test bars of parallel faces, which are usually more challenging to fabricate. For each composition, 10 sintered discs were tested by using a universal testing machine (Instron 4204, Instron, Danvers, Ma, USA). The microstructure of sintered samples was investigated by means of optical (LM Zeiss, Primo Vert, Germany) and scanning electron microscopy (SEM, Quanta FEI 200, Netherlands). 3. Results and discussions The XRD patterns of the waste mixtures, after firing in different conditions, are reported in Fig. 1. As a general trend, the main peaks can be divided into two groups, labeled as “S” and “P” (Fig. 1a and b), each one attributable to a distinct type of compound. While “S” peaks are due to the contribution of silicate phases, such as diopside (CaMgSi2O6, PDF#83-1818) and wollastonite (β-CaSiO3, PDF#72-2284), “P” peaks are due to a phosphate phase, i.e. hydroxyapatite (HAp, PDF#860740). Silicates and phosphates are associated also to minor peaks, attributed to akermanite (Ca2MgSi2O7, PDF#87-0049), tricalcium phosphate (Ca3(PO3)2, PDF#70-2065) and Na–Ca phosphate (NaCaPO3, PDF#74-1950). The “P” peaks are almost constant, in terms of intensity; whereas “S” peaks are quite variable. For A samples (Fig. 1a), “S” peaks decrease when passing from the fast firing treatment (AF, 950 1C for 1 min, after rapid heating) to slow heating treatment (AS, 950 1C for 3 h, after slow heating). Interestingly, for B samples (Fig. 1b), “S” peaks exhibit an opposite trend. Finally, the most crystallized samples for the two
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P
S
S P
Silicates
P P
Akermanite [87-0049] Diopside [83-1818] Wollastonite [72-2284]
AH
BS
Intensity / a.u.
Intensity / a.u.
AS
BH
Intensity / a.u.
S
S
BS Phosphates
HAp [87-0049] Na-Ca phopshate [74-1950] TCP [70-2065]
AF BF
AF
15 20 25 30 35 40 45 50 55 60 65 70 75
15 20 25 30 35 40 45 50 55 60 65 70 75
2θ / deg.
2θ / deg.
15 20 25 30 35 40 45 50 55 60 65 70 75
2θ / deg.
Fig. 1. XRD patterns of (a) A samples and (b) B samples fired in the different conditions; (c) BS and AF, the two most crystallized samples.
Table 3 Physical and mechanical characteristics of the sintered samples. Sample
Density, ρ (g/cm3)
Strength, sf (MPa)
Specific strength sf/ρ (MPa cm3/g)
AF AH AS BF BH BS
1.8 70.7 2.0 70.2 2.0 70.3 2.0 70.3 2.0 70.2 2.0 70.1
18.472.4 12.970.7 14.071.0 7.9 71.80 14.071.0 15.070.5
10.8 6.6 7.2 4.4 7.2 7.7
formulations, AF and BS (Fig. 1c), present an almost similar phase composition. Phosphates phases correspond to unreacted MBM waste; the absence of meaningful variations, comparing A and B samples, is consistent with the fact that the two formulations have the same amount of MBM. Furthermore, the different balance in both A and B formulations between BW and soda-lime glass has an impact on the crystallization of the mixtures. The higher content of soda-lime glass, present in A samples, promotes a substantial crystallization in short firing times, likely attributable to interaction between glass and CaO and MgO oxides from BW; longer firing treatments; AS, evidently favor some dissolution of the silicates, operated by secondary components of the same BW. On the contrary, a lower content of soda-lime glass, present in B samples, promotes a progressive crystallization with a slower thermal cycle. For A samples, the density values slowly increased with the holding time at 950 1C, as reported in Table 3. Considering the slight changes in the crystallization behavior, the difference in density may be interpreted only as a consequence of a different composition and physical characteristics of the developing viscous flow during sintering. SEM observations (Fig. 2) indicate that sample AF presents a much higher porosity in comparison with AH and AS samples, with pores characterized by a quite irregular shape as an effect of crystallization and pore coalescence. Such pores were likely associated to the release of CO2, from the decomposition of calcite (present in BW), and its entrapment in the pyroplastic mass determined by
the viscous flow sintering of the other components. The entrapment was favored by the relatively high heating rate (there was no specific holding stage at 850 1C, that could be considered a starting point for substantial calcite decomposition) [40] and by the partial crystallization, i.e. formation of Ca-rich silicates from interaction between CaO (other product of calcite decomposition) and glass, causing an increase of viscosity. The reduced pore size of sample AH is expected due to enhanced viscous flow of the residual glass phase, the holding time being increased from 1 min to 1 h, with large pores collapsing into smaller ones. Sample AS is obviously denser, since a further enhanced viscous flow, due to a holding time prolonged to 3 h, was combined with a limited entrapment of gas, due to the reduced heating rate. The high magnification details, shown in Fig. 2d–f, confirm a rather high crystallization level, for all three thermal cycles, inferred from XRD analysis. For the B samples, the density values were similar, as presented in Table 3. No large differences in terms of porosity, essentially closed pores, are observed between BF and BH samples (Fig. 3a and b), the microstructure of sample BS (Fig. 3c) is characterized by a diffuse and relatively large interconnected porosity. Backscattered SEM images of a polished surface of BH sample (Fig. 3d and e) show a homogeneous distribution of wollastonite elongated crystals and diopside crystals, mainly located inside the pores (Fig. 3f). The diametral compression strength of sintered samples ranged between 7.887 1.80 for BF sample and 18.40
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Fig. 2. SEM micrographs of: (a and d) AF, (b and e) AH and (c and f) AS samples.
Fig. 3. SEM micrographs of: (a) BF, (b) BH and (c) BS samples; (d–f) high magnification details of sample BH.
7 2.4 MPa for sample AF. These values are in agreement with other silicate waste based glass-ceramics produced earlier, [31–34] and they are quite interesting for the associated density data, with densities lower than 2.1 g/cm3. In particular,
the best results in terms of specific strength (strength to density ratio) correspond to samples with an enhanced crystallization tendency, i.e. more prone to the formation of new crystal phases by reaction among the components. Although the
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diametral compression strength test does not provide the exact flexural or tensile strength of the samples, it does yield a suitable parameter to compare the strength of different materials and it was chosen in this study as previous investigations on sintered waste derived glass-ceramics have used it (e.g. Ref. [41] ). Sample AF, subjected to the simplest and most rapid thermal treatment (fast heating and cooling, limited holding time), may be recognized as the most promising glass-ceramic with a specific strength exceeding 10 MPa cm3/g. Certainly long firing treatments generally cause some densification, but they do not improve significantly the mechanical strength.
4. Conclusions Respecting to the B2O3–P2O5–SiO2 glass-ceramic ternary system, for the first time, glass-ceramics were obtained from a combination of three industrial wastes such as (i) boron waste, (ii) meat bone and meal ash and (iii) soda lime silica glass waste. The influence of rapid sintering, particle sizes of the selected wastes, amount of the glass-ceramic forming oxides and sintering cycle were found to be significant regarding the microstructure evolution and mechanical properties of the produced glass-ceramics. The boron base components act as a flux, providing a liquid phase at about 950 1C which enables densification. The reaction among MgO and CaO together with the silicate phase leads to crystallization of wollastonite and diopside. Sample AF, subjected to the most rapid thermal treatment, may be recognized as the most promising glassceramic, with a specific strength exceeding 10 MPa cm3/g.
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CERAMICS INTERNATIONAL
Ceramics International 40 (2014) 6045–6051 www.elsevier.com/locate/ceramint
Development of glass-ceramics from boron containing waste and meat bone ash combinations with addition of waste glass B. Ciceka,e,n, A. Tuccib, E. Bernardoc, J. Willd, A.R. Boccaccinid a Eczacıbaşı Building Products Co. VitrA Innovation Center, Turkey Department of Biomedical Science and Neuromotor Sciences, University of Bologna, Italy c Department of Industrial Engineering, University of Padova, Italy d Department of Materials Science and Engineering, University of Erlangen-Nuremberg, Germany e Centro Ceramico Bologna, University of Bologna, Italy b
Received 24 September 2013; received in revised form 11 November 2013; accepted 12 November 2013 Available online 20 November 2013
Abstract Glass-ceramic materials represent a great resource for environmental cleanup, because they can stabilize pollutants by vitrification and, at the same time, they may present remarkable mechanical and functional properties enabling novel applications. In this paper, different mixes of three different industrial wastes, namely boron waste (BW), meat bone and meal ash (MBM) and recycled soda lime silica glass (SLG) were prepared by considering the combined effects of thermal cycle requirement, particle sizes of the selected wastes and amount (content) of boron waste. Glass-ceramics were prepared from selected waste mixtures and the physical and mechanical properties of the obtained glass-ceramics were measured. The results underline that boron containing waste-derived glass-ceramics are attractive for applications as gas concrete blocks or as an additive in new generation insulation ceramics. & 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved. Keywords: Glass-ceramics; Borates; Waste recycling; Recycled glass; Building materials
1. Introduction Glass-ceramic materials feature a great potential for environmental cleanup, since they may combine waste stabilization and valorization [1,2]. The stabilization of pollutants is provided by vitrification, i.e. the formation of waste-derived glasses with significant durability, whereas valorization process comes from the controlled crystallization, leading to remarkable mechanical and functional properties of glass-ceramics [3,4]. Glass-ceramics derived from glasses obtained from a variety of wastes, e.g. metallurgical slags [5,6], residues from urban incinerations [7–9], coal ash from power stations [10], or mixtures of them, have been widely reported in the literature [1–4]. The high costs and energy consumption associated to the typical vitrification/ceramization process, however, still constitute an open issue. A possible solution, to be considered n Corresponding author. Eczacıbaşı Building Products Co. VitrA Innovation Center, Bozuyuk/Bilecik, Turkey. Tel.: þ 90 22 83140400; fax: þ90 22 83140412. E-mail address: [email protected] (B. Cicek).
especially for not particularly toxic wastes, comes from a substantial revision of the concept of glass-ceramics, based on direct sintering of inorganic waste, i.e. on a process resembling that of traditional ceramics. With a proper selection of the starting waste, a significant amount of liquid phase may form upon firing and later convert into a glass [11]. This glass may incorporate crystals from unreacted starting materials, as well as newly formed crystals [1,12]. In this paper we referred to combinations of three different industrial wastes, chosen to generate compositions belonging to the B2O3–P2O5–SiO2 (boro-phospho-silicate) ternary system, known to yield interesting glass and glass-ceramics for different functional applications (e.g. dielectrics) [13–15]. The durability of glasses of this system is quite poor, [14] but it may be substantially improved after crystallization by applying different heating rates [16]. The considered industrial wastes consisted of boron waste (BW), meat bone and meal ash (MBM) and recycled soda lime silica glass (SLG). Boron waste (also known as borate waste/boron containing waste), the source of which is essentially the extractive activity
0272-8842/$ - see front matter & 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved. http://dx.doi.org/10.1016/j.ceramint.2013.11.054
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(concentrator waste), has a rather broad phase composition [12]. Even if many studies underline that boron wastes can be used as additives in cement, [17] brick [18] and in the ceramic [19] production, to the authors' knowledge no industrial process, allowing an efficient use of large amounts of boron wastes, is available. The barrier in front of industrial utilization might be the operational difficulties. B-containing wastes have been already proposed to prepare glass ceramics [20–22]. Meat bone and meal ash (MBM), phosphate containing waste, are obtained by crushing bones and meats coming from slaughterhouses, that have no EU legislative approved hazardous compounds, such as brain, spinal cord or diseased animal waste (safe animal waste) and processing them in compliance with the regulatory codes [23,24]. MBM ash is obtained after heat processing the MBM wastes at 800–900 1C and removing all the organic substances, such as proteins. Usually, 100– 320 kg of MBM ash is obtained from a ton of MBM [25]. In European Union countries, especially in England and France, there are high-capacity MBM incineration plants. In France, the obtained MBM is burned together with coal at the rate of 45% to have clinker and the rest (1040 ktons) is reserved for future processes, still to be explored. [25] Soda lime silica glass (SLG) waste is one of the most important waste materials considering its production amount [27]. SLG is collected from windowpanes, bottles (containers), and glass products through various industries (glass packaging and other waste glass residues from municipal, commercial or industrial sources, mixed municipal solid waste and bulky waste etc.). In 2009, 11.5 million tons of packaging glass waste were collected from 27 E.U. countries, including Norway, Switzerland and Turkey. The packaging glass recycle ratio is 65% in EU countries [26] Many investigations have been carried out on the re-use possibilities of waste glasses, especially when glasses are colored and, therefore, hard to separate. Such investigations have generally been focused on utilizing glass residues in
glasses, [28] ceramics, [19,29,30] glass-ceramics, [31] and cements [22]. All these technologies are very attractive, but still need to be extended and further optimization studies are required. The present study aims at evidencing the feasibility of producing glass-ceramics by a combination of the mentioned wastes, applying low cost direct sintering treatments, in turn featuring high heating rates and relatively low maximum temperatures, with a specific attention to the stabilization of the toxic components such as high amount of Boron, possibly embedded in the starting materials, at the lowest possible energy consumption.
2. Experimental procedure 2.1. Materials and processing A colemanite enrichment tailing waste, from Eti Bor Bigadiç deposit (open pit), located in the Marmara region in Turkey, was used as boron waste (BW). The MBM ash was obtained from the Glanford Power Station (Scunthorpe, UK). SLG, provided by SASIL Life (Biella, Italy), was derived from municipal recycling with an off white color. The chemical composition of these wastes, determined with inductively coupled plasma optical emission spectroscopy (ICP-OES model 3200 XL Perkin Elmer, USA), is reported Table 1. The phase composition of the starting material and of the studied mixtures, after the thermal treatments, was determined by X-ray powder diffraction analysis (Philips PW3830, NL); phase identification was achieved by means of the Match! program package (Crystal Impact GbR, Bonn, Germany), supported by data from PDF-2 database (ICDD-International Centre for Diffraction Data, Newtown Square, PA). The thermal characterization of the starting materials was performed with the
Table 1 Chemical and mineralogical composition of used waste materials. BW Chemical composition, in oxides (wt%) 16.1 SiO2 0.2 Na2O K2O 0.5 MgO 6.9 CaO 26.4 SrO 1.2 Al2O3 0.9 Fe2O3 0.1 SO3 P2O5 B2O3 19.7 L.O.I. 28.0
MBM
SLG
2.3 8.7 3.5 1.3 46.4
71.6 13.5 0.4 3.9 9.0
0.2
1.0 0.1
3.6 34.0
Phase composition Calcite Colemanite Olshanskyte Ca Borate Hydrate
Hydroxyapatite Tricalcium phosphate
Amorphous phase
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Table 2 Details of the adopted combinations of formulation and heating rates. Mix
Sample
Heating rate 1C/min
Tmax/Holding time
Cooling
A
AF AH AS
16.5 16.5 2.6
950 1C/1 min 950 1C/1 h 950 1C/3 h
Fast, 1 h Fast, 1 h Slow, natural cooling
B
BF BH BS
16.5 16.5 2.6
950 1C/1 min 950 1C/1 h 950 1C/3 h
Fast, 1 h Fast, 1 h Slow, natural cooling
use of a heating microscopy (Expert System Solutions-Heating microscope HSM, IT). Two different mixtures were prepared. The first one, labeled A, contained 30 wt% of MBM, 30 wt% of BW and 40 wt% of SLG. Due to the presence, in BW, of crystalline phases, such as calcite (CaCO3) and colemanite (CaO 3B2O3 5H2), that released gases during the following heating step, the BW material was calcined at 500 1C. The calcined BW and MBM ash were milled to particle size o 200 mm. SLG was milled to particle size o 150 mm (Retcsh PM 100, Germany), as measured with a laser granulometer. Compared to the annual production amounts and re-use capacities of the selected wastes, BW is the most abundant one. For this reason, in the second studied composition, labeled “B”, always respecting the glass-ceramic ternary system, the amount of BW was increased up to its highest possible limit. As a result, B samples contained 40 wt% of BW and 30 wt% of MBM ash and SLG. It is known that colemanite (CaO 3B2O3 5H2O), present in the used BW, decomposes with the release of five molecules of H2O between 400 and 500 1C, by transforming into a fine particulate material, less than o 200 mm in size [35]. The temperature of onset of dehydration for colemanite is 262 1C and the first water molecule is lost at 327 1C, which coincides approximately with the onset of decrepitating. The last crystal water loss takes place at 412 1C [36]. Several studies underline that the calcination step of colemanite has an effect similar to a milling process [36]. With the aim to set up a production system for glass-ceramics, characterized by low energy consumption, the calcination step of the BW waste, used in B samples, was substituted by milling into finer particle size (o 80 mm). Sintering tests were performed on compacted powder specimens, uniaxially pressed in form of discs of 10 mm diameter and 4.5 mm in height, under a load of 50 kN. Specimens of both mixtures were sintered at 950 1C by using different heating rates. A fast sintering process was used, characterized by a heating rate of 16.5 1C/min up to the maximum heating temperature of 950 1C. The sintered samples are labeled “F”. The samples fired with the same heating cycle, but with 1 h of holding time at 950 1C, are labeled “H”. A rather rapid cooling from the sintering temperature was adopted for both sintering schedules, e.g. it took 1 h to reach room temperature. A slow sintering process was also used for comparison purposes. The heating rate was 2.5 1C/min up to the maximum
temperature of 950 1C, with 3 h of holding time followed by natural cooling. The samples sintered according to this schedule are labeled “S”. The details of the different sintering treatments are summarized in Table 2. 2.2. Mechanical and microstructural characterization The bulk density of fired materials was determined by their weight and volume determination. The mechanical strength of the different sintered samples was measured by the Brazilian test method [37,38]. This method is also known as “diametral compression” and “indirect (splitting) tensile test”, and it is used as an indirect experimental method to measure the tensile strength of materials [39]. One reason to select the Brazilian test method is that it employs samples of simple form (disc shape) as opposed to the flexural strength text which requires prismatic test bars of parallel faces, which are usually more challenging to fabricate. For each composition, 10 sintered discs were tested by using a universal testing machine (Instron 4204, Instron, Danvers, Ma, USA). The microstructure of sintered samples was investigated by means of optical (LM Zeiss, Primo Vert, Germany) and scanning electron microscopy (SEM, Quanta FEI 200, Netherlands). 3. Results and discussions The XRD patterns of the waste mixtures, after firing in different conditions, are reported in Fig. 1. As a general trend, the main peaks can be divided into two groups, labeled as “S” and “P” (Fig. 1a and b), each one attributable to a distinct type of compound. While “S” peaks are due to the contribution of silicate phases, such as diopside (CaMgSi2O6, PDF#83-1818) and wollastonite (β-CaSiO3, PDF#72-2284), “P” peaks are due to a phosphate phase, i.e. hydroxyapatite (HAp, PDF#860740). Silicates and phosphates are associated also to minor peaks, attributed to akermanite (Ca2MgSi2O7, PDF#87-0049), tricalcium phosphate (Ca3(PO3)2, PDF#70-2065) and Na–Ca phosphate (NaCaPO3, PDF#74-1950). The “P” peaks are almost constant, in terms of intensity; whereas “S” peaks are quite variable. For A samples (Fig. 1a), “S” peaks decrease when passing from the fast firing treatment (AF, 950 1C for 1 min, after rapid heating) to slow heating treatment (AS, 950 1C for 3 h, after slow heating). Interestingly, for B samples (Fig. 1b), “S” peaks exhibit an opposite trend. Finally, the most crystallized samples for the two
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P
S
S P
Silicates
P P
Akermanite [87-0049] Diopside [83-1818] Wollastonite [72-2284]
AH
BS
Intensity / a.u.
Intensity / a.u.
AS
BH
Intensity / a.u.
S
S
BS Phosphates
HAp [87-0049] Na-Ca phopshate [74-1950] TCP [70-2065]
AF BF
AF
15 20 25 30 35 40 45 50 55 60 65 70 75
15 20 25 30 35 40 45 50 55 60 65 70 75
2θ / deg.
2θ / deg.
15 20 25 30 35 40 45 50 55 60 65 70 75
2θ / deg.
Fig. 1. XRD patterns of (a) A samples and (b) B samples fired in the different conditions; (c) BS and AF, the two most crystallized samples.
Table 3 Physical and mechanical characteristics of the sintered samples. Sample
Density, ρ (g/cm3)
Strength, sf (MPa)
Specific strength sf/ρ (MPa cm3/g)
AF AH AS BF BH BS
1.8 70.7 2.0 70.2 2.0 70.3 2.0 70.3 2.0 70.2 2.0 70.1
18.472.4 12.970.7 14.071.0 7.9 71.80 14.071.0 15.070.5
10.8 6.6 7.2 4.4 7.2 7.7
formulations, AF and BS (Fig. 1c), present an almost similar phase composition. Phosphates phases correspond to unreacted MBM waste; the absence of meaningful variations, comparing A and B samples, is consistent with the fact that the two formulations have the same amount of MBM. Furthermore, the different balance in both A and B formulations between BW and soda-lime glass has an impact on the crystallization of the mixtures. The higher content of soda-lime glass, present in A samples, promotes a substantial crystallization in short firing times, likely attributable to interaction between glass and CaO and MgO oxides from BW; longer firing treatments; AS, evidently favor some dissolution of the silicates, operated by secondary components of the same BW. On the contrary, a lower content of soda-lime glass, present in B samples, promotes a progressive crystallization with a slower thermal cycle. For A samples, the density values slowly increased with the holding time at 950 1C, as reported in Table 3. Considering the slight changes in the crystallization behavior, the difference in density may be interpreted only as a consequence of a different composition and physical characteristics of the developing viscous flow during sintering. SEM observations (Fig. 2) indicate that sample AF presents a much higher porosity in comparison with AH and AS samples, with pores characterized by a quite irregular shape as an effect of crystallization and pore coalescence. Such pores were likely associated to the release of CO2, from the decomposition of calcite (present in BW), and its entrapment in the pyroplastic mass determined by
the viscous flow sintering of the other components. The entrapment was favored by the relatively high heating rate (there was no specific holding stage at 850 1C, that could be considered a starting point for substantial calcite decomposition) [40] and by the partial crystallization, i.e. formation of Ca-rich silicates from interaction between CaO (other product of calcite decomposition) and glass, causing an increase of viscosity. The reduced pore size of sample AH is expected due to enhanced viscous flow of the residual glass phase, the holding time being increased from 1 min to 1 h, with large pores collapsing into smaller ones. Sample AS is obviously denser, since a further enhanced viscous flow, due to a holding time prolonged to 3 h, was combined with a limited entrapment of gas, due to the reduced heating rate. The high magnification details, shown in Fig. 2d–f, confirm a rather high crystallization level, for all three thermal cycles, inferred from XRD analysis. For the B samples, the density values were similar, as presented in Table 3. No large differences in terms of porosity, essentially closed pores, are observed between BF and BH samples (Fig. 3a and b), the microstructure of sample BS (Fig. 3c) is characterized by a diffuse and relatively large interconnected porosity. Backscattered SEM images of a polished surface of BH sample (Fig. 3d and e) show a homogeneous distribution of wollastonite elongated crystals and diopside crystals, mainly located inside the pores (Fig. 3f). The diametral compression strength of sintered samples ranged between 7.887 1.80 for BF sample and 18.40
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Fig. 2. SEM micrographs of: (a and d) AF, (b and e) AH and (c and f) AS samples.
Fig. 3. SEM micrographs of: (a) BF, (b) BH and (c) BS samples; (d–f) high magnification details of sample BH.
7 2.4 MPa for sample AF. These values are in agreement with other silicate waste based glass-ceramics produced earlier, [31–34] and they are quite interesting for the associated density data, with densities lower than 2.1 g/cm3. In particular,
the best results in terms of specific strength (strength to density ratio) correspond to samples with an enhanced crystallization tendency, i.e. more prone to the formation of new crystal phases by reaction among the components. Although the
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diametral compression strength test does not provide the exact flexural or tensile strength of the samples, it does yield a suitable parameter to compare the strength of different materials and it was chosen in this study as previous investigations on sintered waste derived glass-ceramics have used it (e.g. Ref. [41] ). Sample AF, subjected to the simplest and most rapid thermal treatment (fast heating and cooling, limited holding time), may be recognized as the most promising glass-ceramic with a specific strength exceeding 10 MPa cm3/g. Certainly long firing treatments generally cause some densification, but they do not improve significantly the mechanical strength.
4. Conclusions Respecting to the B2O3–P2O5–SiO2 glass-ceramic ternary system, for the first time, glass-ceramics were obtained from a combination of three industrial wastes such as (i) boron waste, (ii) meat bone and meal ash and (iii) soda lime silica glass waste. The influence of rapid sintering, particle sizes of the selected wastes, amount of the glass-ceramic forming oxides and sintering cycle were found to be significant regarding the microstructure evolution and mechanical properties of the produced glass-ceramics. The boron base components act as a flux, providing a liquid phase at about 950 1C which enables densification. The reaction among MgO and CaO together with the silicate phase leads to crystallization of wollastonite and diopside. Sample AF, subjected to the most rapid thermal treatment, may be recognized as the most promising glassceramic, with a specific strength exceeding 10 MPa cm3/g.
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