Physical Properties of Cenosphere
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PHYSICAL PROPERTIES OF CENOSPHERE A Thesis submitted in partial fulfilment of the requirements for the award of the Degree of Master of Technology in Geotechnical Engineering Civil Engineering Department by SUBHARJIT SEN 212CE1063 DEPARTMENT OF CIVIL ENGINEERING NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA - 769008 MAY 2014 I PHYSICAL PROPERTIES OF CENOSPHERE A Thesis submitted in partial fulfilment of the requirements for the award of the Degree of Master of Technology in Geotechnical Engineering Civil Engineering Department by SUBHARJIT SEN 212CE1063 Under the guidance of Prof. Chittaranjan Patra DEPARTMENT OF CIVIL ENGINEERING NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA - 769008 MAY 2014 II Department of Civil Engineering National Institute of Technology Rourkela – 769008 Odisha, India www.nitrkl.ac.in CERTIFICATE This is to certify that the thesis entitled “Physical Properties of Cenosphere” submitted by Mr. Subharjit Sen (Roll No. 212CE1063) in partial fulfilment of the requirements for the award of Master of Technology Degree in Civil Engineering with specialization in Geo-Technical Engineering at National Institute of Technology, Rourkela is an authentic work carried out by him under my supervision and guidance. To the best of my knowledge, the matter embodied in the thesis has not been submitted to any other University / Institute for the award of any Degree or Diploma. Date: Dr. C R Patra Place: Professor Department of Civil Engineering National Institute of Technology Rourkela – 769008 III Acknowledgment I am heartily thankful to my supervisor, Dr. C.R.Patra, whose encouragement, supervision and support from the preliminary to the concluding level enabled me to develop an understanding of the subject. I cannot fully express my gratitude to the exceptional team at Department of Civil engineering, NIT Rourkela including my friends. I am really thankful to Dr. Dillip KumarPradhan, for his generosity, faith and superb guidance. I extend my thanks to Ph.D. scholars Mr. Satya Narayan Tripathy, Mr. Tapabrata Dam, Mr. Ashutosh Pattanaik and Mr. Sumanta Kumar Sahoo for their co-operation. For the generous assistance in the research of this project, I would like to acknowledge the Department of Metallurgical and Material Science for providing the required lab set up for my sample preparation, Department of Physics for required slot for dielectric measurement and XRD and Department of Ceramics engineering for FESEM. Lastly, I express my deepest gratitude to my parents, brother and my friends for their moral support and love. Subhrajit Sen Roll No-212ce1063 Department of Civil engineering NIT, Rourkela Rourkela-769008 IV Content Pages І.Chapter-1: Introduction 1.1: What is Cenosphere? 1 1.2: Uses of cenosphere 2 1.3: Constituents of cenosphere 4 1.4: Thermal Analysis 5 1.4.1: Uses of Thermal Analysis Techniques 5 1.4.2: Thermal Analysis Instruments 6 1.4.3: Thermogravimetry 7 1.4.4: Presentation of TGA data 7 1.4.5: Instrumentation of Thermal analyser 7 1.4.6: The Thermobalance 8 1.4.7: Differential Thermal Analysis (DTA) 8 1.4.8: Data Presentation 10 1.4.9: Reference Materials 10 1.5: Electrical resistivity 11 1.5.1: Origin of resistance 11 1.5.2: Resistivity 11 1.5.3: Resistivity measurement methods 12 1.5.4: Two probe method 12 1.5.5: Dielectric constant 12 1.5.6: Loss tangent 12 ІІ.Chapter-2: Literature study and Objective 2.1: Literature study 15 2.2: Main objective 18 ІІІ.Chapter-3: Experimental Technique 3.1: Sample Preparation 19 3.1.1: Why these chemicals are used in the cleaning process? 20 3.1.2: Why ultrasonication is required in the sample synthesis? 21 3.2: Particle size distribution 21 3.3: Specific surface area 23 3.4: Compressive strength 25 3.5: Compositional analysis 26 3.6: X-ray diffraction (XRD) 28 3.7: Field emission scanning electron microscope 30 3.8: Energy dispersive X-ray spectroscopy (EDS) 30 3.9: Thermal Analysis 31 3.10: Dielectric Property Measurement 32 ІV.Chapter-4: Results and discussion 4.1: Collection of cenosphere 37 4.2: Particle size analysis 37 4.3: Specific Surface Area 38 4.4: Compaction characteristics 38 4.5: Compositional Analysis 41 4.6: Mineralogical composition 42 4.7: Morphological analysis 45 4.8: EDS of cenosphere 46 4.9: Thermal analysis 47 4.10: Electrical Resistivity and Dielectric spectroscopy 48 V. Conclusion 51 VІ. References 52 Abstract Cenospheres are exclusive free flowing powders comprised of hard shelled, hollow, tiny spheres collected from coal ash. Their amount is based on the C and Fe content present in the fly ash. Due to lower value of thermal conductivity, higher particle strength, ultra-low density, impermeability they are used in various industries. However, it is necessary to study the various physical properties of these ash particles for its improved and effective usage. In the present study, systematic investigation of the structural, microstructural, thermal, electrical and mechanical properties of cenosphere have been carried out. X-ray diffraction studies reveal the primary constituents of cenosphere. Quartz, mullite, sillimanite, magnetite, hematite, rutile, dipotassium oxide, calcium oxide, sodium oxide, magnesium oxide are the primary constituent of cenosphere. FESEM micrographs indicate that cenosphere is a hard shelled hollow space. Plerosphere is also found in the light weight particle. Complex impedance spectroscopy has been employed to analyze the bulk properties of the material. The room temperature dielectric study shows the high electrical resistivity property. The frequency dependent dielectric spectroscopy confirms polar characteristics of cenosphere. The average diameter of cenosphere is around 100μm. TGA and DTA thermogram of cenosphere reveals the higher thermal stability of cenosphere. Cenosphere is stable up to 1000◦C with negligible mass loss. The endothermic peak around 300◦C reveals decomposition of carbonaceous material in cenosphere. Compressive strength of cenosphere has been carried out. Compressive strength of cenosphere pellet produced by 6 ton loading is around 7.38 MPa. I LIST OF FIGURES 1.1: Thermal Analyser 6 3.1: Dynamic Light Scattering Zeta Sizer: Malvern Instrument 22 3.2: Blain‟s air permeability apparatus 25 3.3: Uniaxial Compessive strength testing machine 26 3.4: Dye 26 3.5: Pellets 26 3.6: Bragg‟s reflection from crystallographic planes 29 3.7: Interaction of electron beam with specimen 31 3.8: Phase diagram between current and voltage 33 3.9: Variations of and with frequency 33 3.10: Relationship between microstructure-electrical properties in complex impedance plane and an electrical equivalent circuit in complex impedance plane 35 4.1: Collection of cenosphere 37 4.2: Particle size distribution of cenosphere 38 4.3: Particle size distribution of fly ash 39 4.4: XRD diffraction spectra of cenosphere 43 4.5: XRD diffraction spectra of constituent compounds 43 4.6: XRD diffraction spectra of constituent compounds 44 4.7: XRD diffraction spectra of fly ash 44 4.8: Distribution of cenosphere Matrix 45 4.9: Average size of cenosphere 45 4.10: Cenosphere 46 4.11: Void space of cenosphere 46 4.12: Plerosphere 46 4.13: Thickness of cenosphere diameter 46 4.14: EDS of cenosphere 47 4.15:EDS of Fly ash 47 4.16: TGA and DTA pattern of cenosphere sample 48 4.17: Dielectric permittivity and loss tangent of cenosphere 49 4.18: Electrical resistance and capacitance of cenosphere 49 4.19: Complex impedance and phase angle of cenosphere 50 II LIST OF TABLES 4.1: Compressive Strength for 6 ton cenosphere pellets 40 4.2: Compressive Strength for 4 ton cenosphere pellets 40 4.3: Chemical composition (wt. %) of the cenosphere sample 41 4.4: Chemical composition (wt. %) of the fly ash sample 41 III Chapter-1 Introduction 1 INTRODUCTION 1.1 What is Cenosphere? Coal fired boilers are extensively used to produce steam for production of electricity. A common form of boiler uses a pulverized coal that is injected into a furnace. Fly ash is produced by of burning coal in boiler. Some of the improved fly ash is commercially utilizable in concrete, concrete products, cement production, sewage sludge stabilization, pavement base materials, lightweight aggregate, reinforced plastics, and other miscellaneous purposes. The residual fly ash must usually be disposed of by land filling since it has hardly any commercial value. It is well acknowledged that landfill space is quickly failing in many regions and that the construction of new landfills is very expensive. In this way, much endeavor has been administered at discovering utilization for fly ash remains with the goal that the fly ash does not require to be land filled and any usable item from this waste material is praiseworthy. Depending on the composition of coal the composition of fly ash varies. Therefore, to be used in specific applications material specifications have been developed for this waste material. The particular shows that these waste particles are made for the most part of silicon dioxide, aluminum oxide and iron oxide. Different types of structures are observed in the particles in fly ash. A few particles in fly ash are strong. Different particles in fly ash are empty and are called cenospheres. The expression "cenosphere" is determined from two Greek words, kenos (empty) and sphaira (sphere). Cenospheres are lightweight, idle, and empty circles basically comprising of silica and alumina, are loaded with air or gasses, and are by results of the ignition of pulverised coal at the warm power plants. A cenosphere is a lightweight, idle, empty sphere made to a great extent of silica and alumina and loaded with air or inactive gas, commonly processed as a by-result of coal burning at warm power plants. Cenospheres fluctuates from light black color to practically white shade and their specific gravity extends in the middle of 0.4–0.8 g/cm³, which offers them extraordinary lightness.