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Assessing the Pozzolanic Activity of Cements with Added Sugar Cane Straw Ash by Synchrotron X-Ray Diffraction and Rietveld Analysis ⇑ Guilherme A

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Assessing the Pozzolanic Activity of Cements with Added Sugar Cane Straw Ash by Synchrotron X-Ray Diffraction and Rietveld Analysis ⇑ Guilherme A Construction and Building Materials 98 (2015) 44–50 Contents lists available at ScienceDirect Construction and Building Materials journal homepage: www.elsevier.com/locate/conbuildmat Assessing the pozzolanic activity of cements with added sugar cane straw ash by synchrotron X-ray diffraction and Rietveld analysis ⇑ Guilherme A. Calligaris a, Margareth K.K.D. Franco b, , Laurence P. Aldrige c, Michelle S. Rodrigues d, Antônio Ludovico Beraldo d, Fabiano Yokaichiya b,e, Xavier Turrillas f, Lisandro P. Cardoso a a Universidade Estadual de Campinas (UNICAMP), Instituto de Física Gleb Wataghin (IFGW), 13083-859 Campinas, SP, Brazil b Comissão Nacional de Energia Nuclear (CNEN), Instituto de Pesquisas Energéticas e Nucleares (IPEN), Reator Multipropósito Brasileiro (RMB), Brazil c Institute of Material Engineering, ANSTO, PMB 1 Menai, New South Wales 2234, Australia d Universidade Estadual de Campinas (UNICAMP), Faculdade de Engenharia Agrícola (FEAGRI), Campinas, SP, Brazil e Helmholtz-Zentrum Berlin für Materialien und Energie (HZB), Germany f Consejo Superior de Investigaciones Científicas, Institut de Ciència de Materials de Barcelona, Spain highlights Sustainability is the key word in the development of new technologies. The use of alternative materials in the cement paste is focused. Cement pastes and cement pastes blended with Sugar Cane Straw Ashes were studied. Our findings contribute in the phase identifications of cementitious pastes. The pozzolanicity of the agroindustrial wastes was proven using synchrotron radiation. article info abstract Article history: Sugar and alcohol industries generate large amount of wastes that could produce ashes of great reactivity Received 6 June 2014 with pozzolan properties. The objective of this paper is to evaluate the pozzolanicity of Sugar Cane Straw Received in revised form 7 August 2015 Ashes (SCSA), thermal treated, at different curing times. Employing Synchrotron X-ray radiation for XRD Accepted 10 August 2015 measurements, scans from 10 to 110 (h À 2h setup) allowed the quantification of several phases of the Available online 24 August 2015 cement pasts through Rietveld analysis. The SCSA substitution of 20% (weight) in Ordinary Portland Cement (OPC) has improved the AFt (Ettringite) formation up to 47% for 90 days curing time. The Keywords: Portlandite concentration analysis allowed concluding that this addition of SCSA in OPC has caused a Synchrotron radiation characterisation delay in the cement setting time. Moreover, the behaviour of the C3S and Calcite contents in both OPC Sugar cane straw ash Pozzolan and OPC/SCSA samples were determined by refinement of the XRD pattern using the Rietveld method. Waste management Ó 2015 Elsevier Ltd. All rights reserved. 1. Introduction and also by the use of biomass for power generation. Despite these mitigating factors, the expansion of construction activity in Brazil Industrial production of cement in Brazil started in 1920, reach- motivates the search for materials that can replace cement. This ing a maximum of 40.2 million tones in 1999 [1]. Despite of a series replacement is necessary due to the environmental and social of up and downs due to economic upheaval, another peak of 65 impacts caused by the production of cement. million tons was attained in 2011. Preliminary information about Researches involving the use of pozzolans in cementitious cement consumption on April 2013 reached 5.9 million of tons [2]. matrices have increased significantly in recent years. In the Nowadays, the Brazilian cement industry is among the 10 absence of natural pozzolan, cement industries look for new mate- largest cement world producers and consumers, has a modern rials in agroindustry. Several authors have reported the use of industrial park, is internationally recognised for recycling waste agroindustrial ashes to partially replace Portland cement [3–7]. minerals and by preserving the environment (low CO2 emissions) The use of sugar cane straw, as forage, contributes to decrease the soil erosion and to reduce the carbon emission from soil to ⇑ atmosphere [8]. Furthermore, the wastes of sugar cane production Corresponding author. can be recycled by biorefinaries to get energy with a substantial E-mail address: [email protected] (M.K.K.D. Franco). http://dx.doi.org/10.1016/j.conbuildmat.2015.08.103 0950-0618/Ó 2015 Elsevier Ltd. All rights reserved. G.A. Calligaris et al. / Construction and Building Materials 98 (2015) 44–50 45 generation of ashes. Since Brazil is the world’s largest producer of 2.1.2. Ordinary Portland Cement (OPC) and OPC/SCSA sugar cane having a huge organic by-products surplus of bagasse The highly initial resistance cement, Ordinary Portland Cement and straw [8,9] has a strong interest in finding a way to recycle this (OPC), (CPV-ARI, Cauê) was utilised in this study, according to the waste. One possible solution could be its combustion. Indeed, some ABNT NBR 5733 (1991) [15]. This cement does not show mineral authors have reported that these wastes when burned under additions. On the other hand it shows higher quantities of C3S controlled temperature may show high reactivity, reacting as a and C2S than others, resulting more reactivity. It was prepared pozzolanic material [10,11]. two pastes, the control (pure OPC) and OPC/SCSA (80%/20% by To assess a pozzolanic material it is necessary to carry out a weight). OPC, without mineral addition, calcium hydroxide (95% complete series of chemical, physical and mechanical tests to eval- of purity) and deionised water were used in blended cement uate its performance. One of them involves the direct identification pastes. Firstly, OPC and ash was mixed and then it was added deio- of calcium silicate hydrates (CSH) phases, promoted by pozzolanic nised water; the water/binder ratio was 0.5. After mixing the mate- reaction, as a function of time [12–14] up to ninety days. This can rials, pastes were stored in sealed plastic bottles and then left in a be carried out by X-ray diffraction, quantifying both the initial curing room at 20 C until the tests applied. At ages test manual crystalline phases and the hydration products over long periods grinding pulverised the samples. The hydration of the samples (months), since the pozzolanic reaction is normally slow. was stopped by putting the samples into an acetone solution. The aim of this paper, consequently, is to evaluate the poz- Afterward, samples were dried at 60 °C for 30 min in furnace. zolanic reaction in blended cement pastes, both without (control) and with sugar cane ashes added, treated at 700 C, for periods of 2.2. Experimental characterisation techniques three, seven, twenty-eight and ninety days. To achieve that, syn- chrotron X-ray diffraction data acquired at the Brazilian facilities 2.2.1. SCSA of LNLS, have been studied and crystalline phases quantified by The chemical composition of the ash was determined using the Rietveld analysis in order to have a picture of the major phases X-ray fluorescence method, Axios from Panalytical, and the loss on evolution during the cement pastes hydration. ignition (LOI) was measured according with ASTM C 114 method [16]. X-ray diffraction (XRD) of SCSA was performed at D10B- XPD [17] and D12A-XRD1[18] in the Brazilian Synchrotron 2. Experimental procedure Laboratory (LNLS) using 4 + 2-circle Huber diffractometers in a high-resolution mode, with Ge 111 analyser crystal, at 8 keV. 2.1. Materials This mode was chosen in order to minimise the superposition of neighbouring Bragg peaks allowing for more reliable solution of 2.1.1. Sugar Cane Straw Ashes (SCSA) the mineralogical characterisation. Data were obtained at room The sugar cane straw was harvested from Centro de Tecnologia temperature, in a h À 2h geometry (Bragg–Brentano configuration), Canavieira (CTC), placed at Piracicaba, São Paulo – Brazil. It was col- with a flat plane sample holder, over a 2h range of 10–70° with a lected directly from the ground and exposed to the natural environ- step size of 0.01° and a step time of 1s. Granulometric distribution ment to naturally dry for 24 h. The ash was obtained from the of Ordinary Portland Cement and ash were measured using a burning control in an electrical furnace with 10 C/min heating rate Malvern Mastersizer 2000 apparatus which allows an analysis of during 3 h at 700 C X(hereafter SCSA). The production of the ashes particles by laser diffraction from 0.02 to 2000 lm in liquid mode was divided in two levels in order to obtain a homogeneous burning, as dispersant, with 10–15% of obscuration and ultrasonic agitation according to Fig. 1. On reaching the first temperature level, 400 C, for 60 s. The fineness of the material is an important parameter to the system remains 20 min in order to burn all the organic matter evaluate the pozzolanicity. Higher the contacts surface of the poz- to get the best homogenisation of the ash. In the second level, the zolan with calcium hydroxide, greater the rate of pozzolanic material was maintained at 700 C for 1 h. At the end, the muffle reaction. furnace was turned off and a slow and natural cooling process began. The muffle furnace model 10013 from Jung, used to treat the sam- ples, has the dimension of 27 cm  40 cm  100 cm. Afterwards, it 2.2.2. Ordinary Portland Cement (OPC) and OPC/SCSA was used a rotor mill from Tecnal to mill the ashes at 200 rpm during Synchrotron X-ray powder diffraction has become a well- 120 min. established technique, being suitable for applications in character- isation of cementicious materials [19,20]. This technique that pre- sents the advantage of large photon flux of a synchrotron source and high resolution compared with the conventional X-ray diffrac- tometers, allow us to evaluate with more accuracy the composition of blend paste cement in different curing time.
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