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Sintering and Mechanical Properties of Alumina-Yttrium Aluminate Composites

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Sintering and Mechanical Properties of Alumina-Yttrium Aluminate Composites SINTERING AND MECHANICAL PROPERTIES OF ALUMINA-YTTRIUM ALUMINATE COMPOSITES A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENT FOR THE DEGREE OF Master of Technology in INDUSTRIAL CERAMICS BY SUDHANSHU RANJAN 213CR2133 DEPARTMENT OF CERAMIC ENGINEERING NATIONAL INSTITUTE OF TECHNOLOGY Rourkela MAY 2015 CERTIFICATE This is to certify that the thesis entitled “SINTERING AND MECHANICAL PROPERTIES OF ALUMINA-YTTRIUM ALUMINATE COMPOSITES” submitted by Mr. SUDHANSHU RANJAN (213CR2133) in partial fulfilment of the requirement for the award of MASTER OF TECHNOLOGY degree in INDUSTRIAL CERAMIC ENGINEERING at the 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 S.BHATTACHARYYA Dept. of Ceramic Engineering National Institute of Technology Rourkela-769008 ACKNOWLEDGEMENT I wish to express my deep sense of gratitude and indebtedness to Prof. S. Bhattacharyya, Department of Ceramic Engineering, N.I.T Rourkela for assigning me the project “SINTERING AND MECHANICAL PROPERTIES OF ALUMINA-YTTRIUM ALUMINATE COMPOSITES” and for his inspiring guidance, constructive criticism and valuable suggestion throughout this project work. I am very thankful to Prof. S. K. Pratihar, Head of The Department, for his cooperation. It would haven’t been possible for me to bring out this project report without his help and constant encouragement. I would like to express to our Prof. J. Bera, Prof. R. Sarkar for their valuable suggestions and encouragements at various stages of the work. I am also thankful to research scholars in Department of Ceramic Engineering for providing all joyful environments in the lab and helping me throughout this project. I would also take this opportunity to express my gratitude to Bapi Sir and Arvind Kumar Sir for their help, and lastly I am thankful to my parents and friends for their constant support. SUDHANSHU RANJAN 213CR2133 INDEX CHAPTER TITLE PAGE NO. NO. ABSTRACT i LIST OF TABLES ii LIST OF FIGURES iii 1 INTRODUCTION 1 2 LITERATURE REVIEW 4 3 EXPERIMENTAL WORK 10 3.1 Powder Processing 11 3.1.1 Synthesis of Yttrium Nitrate 11 3.1.2 Estimation of Yttrium Nitrate solution 11 3.1.3 Preparation of Al2O3 –Y(NO3)2 mix and calcination 12 3.1.4 Compaction and Sintering 12 3.1.5 Processing of Al2O3-YAG Composites 13 3.2 Flow sheet of processing of the Al2O3-YAG Composites. 13 3.3 Characterization 14 3.3.1 Thermal decomposition behaviour of Al2O3 Yttrium 14 Nitrate powder mix 3.3.2 XRD 14 3.3.3 Bulk Density and Apparent Porosity 14 3.3.4 Vickers Hardness 14 3.3.5 Flexural Strength 15 3.3.6 Fracture Toughness 16 3.3.7 Microstructure of Sintered Specimens 17 4 RESULTS AND DISCUSSIONS 18 4.1 Decomposition behaviour of Yttrium Nitrate and 19 Crystallization of Yttrium Aluminate 4.2 Phase evolution in the calcined Al2O3-Y2O3 powder 20 4.2.1 Phase Evolution in Al2O3-40 mol % Y2O3 21 4.2.2 Phase Evolution in Al2O3-50 mol % Y2O3 21 4.2.3 Phase Evolution in Al2O3-60 mol % Y2O3 22 4.3 Phase analysis of sintered Al2O3- Yttrium Aluminate 22 Composites 4.4 Bulk Density and Relative Density of Sintered Alumina 25 as a function of Yttrium Aluminate of Composites 4.5 Apparent Porosity of Sintered Alumina as a function 26 of Yttrium Aluminate of Composites 4.6 Hardness of Sintered Alumina as a function 27 of Yttrium Aluminate of Composites 4.7 Flexural Strength of sintered Alumina as a function 27 of Yttrium Aluminate of Composites 4.8 Fracture Toughness of sintered Alumina as a function 28 of Yttrium Aluminate of Composites 4.9 Microstructure of Sintered Specimen Alumina-YAG 29 Composites 4.10 Microstructure of indented samples of Alumina-YAG 29 Composites 5 CONCLUSIONS 31 REFERENCES 33 ABSTRACT Yttrium Aluminate (having different mole percent of Y2O3) were prepared by mixing of Al2O3 o and Y(NO3)2.6H2O and calcination of powder at 1400 C. The calcined Yttrium Aluminate powder was added to Aluminain different volume fractions (5, 10, 15 and 20 vol%), compacted and sintered at 1650oC. The sintered sample had a relative density (82-90 % of theoretical). The sintered samples were characterised by bulk density, apparent porosity, hardness, strength, toughness and microstructure. The fracture toughness as measured by Indentation Strength in Bending(ISB) method was 2.4 MPa√m for pure Alumina and it increased to 4.21 MPa√m at 20 vol% Yttrium Aluminate addition. Microstructure showed that the Yttrium Aluminate was inhomogeneously distributed in the Alumina matrix. The crack path of the indented samples indicates that crack bowing takes place in Alumina–Yttrium Aluminate samples. It is concluded that proper densification of the composites could possibly further increase the toughness and strength. i LIST OF TABLES S.no Title Page no 4.1 Relative Fraction of Al2O3 and YAG in the Sintered 25 Samples of Alumina- Yttrium Aluminate Composites 4.2 Relative density of Yttrium Aluminate phases in alumina 25 4.3 Fracture toughness of sintered sample at 1650oC 28 ii LIST OF FIGURES S.no Title Page no 3.1 Phase Diagram of Y2O3-Al2O3 System 12 3.2 Flow Diagram for the Processing of the Al2O3-YAG composites 13 3.3 Schematic diagram of Vickers hardness indenter 15 3.4 Schematic diagram of 3-point flexure strength test 16 4.1 DSC/TG, Alumina – 40 mol% Y2O3 (as Yttrium Nitrate) 19 4.2 DSC/TG, Alumina – 50 mol% Y2O3 (as Yttrium Nitrate). 20 4.3 DSC/TG, Alumina – 60 mol% Y2O3 (as Yttrium Nitrate). 20 4.4 XRD pattern of Alumina- 40 Mole % of Y2O3 calcined 21 at different temperature 4.5 XRD pattern of Alumina- 50 Mole % of Y2O3 calcined 21 at different temperature 4.6 XRD pattern of Alumina- 60 Mole % of Y2O3 calcined 22 at different temperature 4.7 XRD pattern of Alumina40 Mole % of Yttrium Aluminate 23 Of Composites 4.8 XRD pattern of Alumina50 Mole % of Yttrium Aluminate 24 of Composites iii 4.9 XRD pattern of Alumina60 Mole % of Yttrium Aluminate 24 of Composites 4.10 Relative density of sintered sample at 1650oC 26 4.11 Apparent Porosity of sintered sample at 1650oC 26 4.12 Hardness of sintered sample at 1650oC 26 4.13 flexural strength of sintered sample at 1650oC 28 4.14 Microstructure of Sintered Alumina-60 Mole % of 29 Yttrium Aluminate 20 vol % Composites 4.15 Crack path in the indented samples (a) Pure Alumina 30 (b) Alumina- 20 vol% YA (40 mol%) 4.16 Crack path in the indented samples (a)Alumina- 20 vol% YA 30 (50 mol%) (b) Alumina- 20 vol% YA (40 mol%) iv Chapter-1 INTRODUCTION 1 Alumina is one among the important ceramic materials both for traditional as well as for advanced applications. Among its diversified application areas, some of the key areas are grinding tubes, crucibles and tubes for high-temperature applications, cutting tool inserts, etc. The properties of Alumina that result in this application are high corrosion and erosion resistance, impact resistance, high-temperature stability. However, low fracture toughness and brittle fracture behaviour of Alumina puts a limitation on the widespread application of alumina. Many methods have been tried to improve the resistance to crack propagation or, in other words, fracture toughness. Ductile metals such as (Cu, Ni) have been added to Alumina in order to impart ductility and higher toughness. This method has resulted in the development of Cu-Alumina and Ni-Alumina composites [1]. The use of TiC in Alumina have not only the toughness and strength but it has also improved the overall thermal conductivity and hence the thermal shock resistance [2]. On the other hand, the combination of Alumina and different Stabilized Zirconia (Y-TZP, Y-PSZ) have also been successful in creating a tough ceramics (ATZ and ZTA). All the ideas discussed above dealt with two distinct phase which are the virtually non-interacting type. The toughness improvement in these above cases result from dispersion strengthening and transformation toughening, respectively. But there are certain other additives like SrO and Y2O3 which when added to Alumina produce the corresponding Aluminate phase (Strontium Aluminate or Yttrium Aluminate respectively) which can also improve the crack propagation resistance [3]. However, the improvement, in this case, can be attributed to the elongated particle morphology that provided the crack bridging effect. Cutler et al had observed that the addition of 15 vol % SrO to Ce-TZP/Al2O3 yielded elongated SrZO3 into in the matrix that improved the strength and toughness [4]. Lach et al [5] reported that Y2O3 addition in Al2O3 results in YAG phase formation that improved the toughness. The toughness increment was due to the higher crack growth resistance of YAG phase. It was also reported by Rana [6] while working on Al2O3-YTZP composite that even a small fraction of 2 YAG could improve the mechanical properties of Al2O3-YTZP. In view of these observations, it was thought that addition of Y2O3 to Alumina for deliberate generation of YAG in situ in Alumin is also expected to affect the densification and the fracture behaviour of the composites. In view of the above facts, it was thought worthwhile to study the following aspects: (a) Study of the effect of different Al2O3-Y2O3 molar ratio on the different Yttrium Aluminate compositions. Normally, YAG is the most desired phase in the Al2O3-Y2O3 system. However, depending on the molar ratio of Al2O3-Y2O3, YAM and YAP (the two other phases of Al2O3-Y2O3) may also form.
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