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http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/79119完整後設資料紀錄
| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 段維新 | |
| dc.contributor.author | Bo-Ting Lu | en |
| dc.contributor.author | 盧柏廷 | zh_TW |
| dc.date.accessioned | 2021-07-11T15:45:30Z | - |
| dc.date.available | 2023-08-10 | |
| dc.date.copyright | 2018-08-10 | |
| dc.date.issued | 2018 | |
| dc.date.submitted | 2018-08-08 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/79119 | - |
| dc.description.abstract | 多晶透光氧化鋁由於其機械性質好、化學及溫度穩定性高，多應用在極端環境，如武裝玻璃、高溫爐視窗等。此外，若在其中作摻雜，則可拓寬其應用，有潛力發展成為雷射介質、閃爍體及發光二極體基板。本研究中，採用不同的成型法(乾壓成形、石膏模注漿成形及壓濾成形)，搭配空氣燒結，製備多晶透光氧化鋁，並比較製程對材料燒結行為、微結構以及直線透光度的影響。實驗結果顯示，由壓濾成形的生胚由於堆疊較均勻，在燒結後擁有最佳的透光度；而使用乾壓成形的生胚，生胚密度較低，且內部可觀察到許多裂縫，並在燒結後無法完全去除孔洞，因此透光性不好；以石膏模注漿成形之試片，推測由於模具碎片剝落並滲入生胚，導致燒結時發生異常晶粒成長，因此透光度也不佳。本研究進一步以壓濾成形法製備摻雜三價銪之透光多晶氧化鋁。發現所需緻密化之燒結溫度上升，且在摻雜量為0.1 at%、於1400C燒結的試片中，可觀察到EuAlO3的二次相析出。摻雜的試片透光度較未摻雜之多晶氧化鋁直線透光度低，且隨著摻雜量上升而下降。 | zh_TW |
| dc.description.abstract | Optical polycrystalline alumina (PCA) is a potential ceramic for the applications in harsh environmental conditions, such as armor window and window for high temperature furnace. It is mainly due to its good mechanical properties, chemical stability and thermal stability. By doping elements, the application can be further extended. In the present study, various forming methods such as die pressing, slip casting with a gypsum mold, and pressure filtration are adopted to prepare the green compacts. The results indicate that the specimens formed by pressure filtration exhibits optimum in-line transmission after sintering in air. Such result can be related to the uniform packing of green compacts. On the other hand, for the specimens formed by die pressing, some cracks are observed in the green compacts, and residual pores still exist after sintering. Debris from the gypsum mold is speculated to induce abnormal grain growth of alumina. Such abnormal grains can only be observed in the specimens formed by slip casting with a gypsum mold. As a result, the specimens formed by die pressing and slip casting are opaque after sintering. Besides, Eu3+ doped PCA is also prepared by pressure filtration. The sintering temperature required to densify the Eu3+ doped PCA specimens is higher. Second phase precipitates of EuAlO3 are detected in the specimen doped with 0.1 at% Eu3+. In-line transmission thus decreases with increasing doping levels. | en |
| dc.description.provenance | Made available in DSpace on 2021-07-11T15:45:30Z (GMT). No. of bitstreams: 1 ntu-107-R05527031-1.pdf: 8792933 bytes, checksum: bce85fe2bc44ba604fa423a3f121a207 (MD5) Previous issue date: 2018 | en |
| dc.description.tableofcontents | 口試委員會審定書 #
誌謝 i 中文摘要 ii ABSTRACT iii CONTENTS iv LIST OF FIGURES vii LIST OF TABLES xii Chapter 1 Introduction 1 Chapter 2 Literature survey 3 2.1 α-Al2O3 (alpha alumina) 3 2.2 Optical polycrystalline alumina (PCA) 6 2.2.1 Transparent ceramics 6 2.2.2 Transmission mechanism of PCA 9 2.2.3 Rare-earth doped PCA 12 2.3 Processing of optical PCA 15 2.3.1 Forming methods 15 2.3.2 Slurry preparation 17 2.3.3 Post-sintering HIP 20 Chapter 3 Experimental Procedures 23 3.1 Starting materials 23 3.1.1 Alumina powder 23 3.1.2 Dispersant 23 3.1.3 Europium dopant 23 3.2 Forming process 24 3.2.1 Die pressing 24 3.2.2 Slip casting with a gypsum mold 24 3.2.3 Pressure filtration 25 3.3 Sintering 26 3.4 Characterization 32 3.4.1 Powder properties 32 3.4.2 Slurry fluidity 32 3.4.3 Green compact properties 32 3.4.4 Dilatometer analysis 33 3.4.5 Microstructure observation of the sintered specimens 33 3.4.6 Relative density 34 3.4.7 Grain size measurement 34 3.4.8 Phase identification 35 3.4.9 In-line transmission 35 Chapter 4 Results 36 4.1 Milling of powder 36 4.2 Preparation of slurry 39 4.3 Properties of green compacts 42 4.3.1 Die pressing 42 4.3.2 Slip casting with a gypsum mold 43 4.3.3 Pressure filtration 43 4.4 Sintering kinetics 45 4.5 Relative density of the sintered specimens 48 4.6 Microstructure of the sintered specimens 49 4.7 Grain size measurement 59 4.8 In-line transmission 60 4.9 Phase analysis 62 4.10 Europium (Ⅲ) doped PCA 63 4.10.1 Sintering kinetics 63 4.10.2 Microstructure of the sintered specimens 64 4.10.3 Relative density and grain size 72 4.10.4 In-line transmission 73 4.10.5 Phase analysis 75 Chapter 5 Discussions 77 5.1 Rheological properties 77 5.2 Green compacts 81 5.3 Sintering behavior and microstructure 83 5.3.1 Pure PCA 83 5.3.2 Europium (Ⅲ) doped PCA 86 5.4 In-line transmission 89 5.4.1 Pure PCA 89 5.4.2 Europium (Ⅲ) doped PCA 91 5.5 General discuss and future work 93 Chapter 6 Conclusions 94 REFERENCE 96 LIST OF FIGURES Fig. 2.1 α-Al2O3 (also called corundum structure) and its top view. The small black dots represent aluminum cations, while the large gray spheres represent oxygen anions. [19] 4 Fig. 2.2 The schematic of the transmission when light passes through an alumina specimen. 12 Fig. 2.3 The schematic of the pressure filtration process for forming a green compact. 17 Fig. 2.4 The schematic of the relation between the dispersant amount and the dispersion of the particles in the suspension. 19 Fig. 2.5 The pressurized gas atoms act like “hot forges” and collide with the surface of the specimen to generate applied pressure during HIP. 21 Fig. 3.1 Flow chart for the specimens formed by die pressing 27 Fig. 3.2 Flow chart for the specimens formed by slip casting with a gypsum mold. 28 Fig. 3.3 Flow chart for the specimens formed by pressure filtration. 29 Fig. 3.4 Dimensions of the gypsum mold. 30 Fig. 3.5 Mold for the pressure filtration process. 30 Fig. 3.6 Pressure profile for the pressure filtration process. 31 Fig. 3.7 Schematic of the in-line transmission measurement. 35 Fig. 4.1 Morphology of the alumina particles (a)before and (b)after planetary ball milling for 4 hours 37 Fig. 4.2 Morphology of the alumina agglomerates (a)before (b)after planetary ball milling for 4 hours 37 Fig. 4.3 Particle size distribution of the alumina particles after planetary ball milling for 4 hours. 38 Fig. 4.4 Apparent viscosity of the slurry with a solid content of 72.6 wt% by adding different amount of D-305. The shear rate used was 425 s-1. 40 Fig. 4.5 Apparent viscosity of the slurry with a solid content of 76.5 wt% by adding different amount of D-305. The shear rate used was 425 s-1. 40 Fig. 4.6 Apparent viscosity of the slurries with a fixed amount of D-305 at 1.75 wt%. The shear rate ranged from 51 s-1 to 425 s-1. 41 Fig. 4.7 Fracture surface of the green compacts formed by die pressing. 42 Fig. 4.8 Fracture surface of the green compacts formed by slip casting with a gypsum mold. 43 Fig. 4.9 Fracture surface of the green compacts formed by pressure filtration under a pressure of (a)0.24 MPa, (b)0.31 MPa, and (c)0.46 MPa. 44 Fig. 4.10 Linear shrinkage and the shrinkage rate of the specimen formed by die pressing during the heating stage up to 1500oC. 46 Fig. 4.11 Linear shrinkage and the shrinkage rate of the specimen formed by slip casting during the heating stage up to 1500oC. 46 Fig. 4.12 Linear shrinkage of the specimens formed by pressure filtration under a pressure of 0.24 MPa, 0.31 MPa, and 0.46 MPa during the heating stage up to 1400oC. 47 Fig. 4.13 Shrinkage rate of the specimens formed by pressure filtration under a pressure of 0.24 MPa, 0.31 MPa, and 0.46 MPa during the heating stage up to 1400oC. 47 Fig. 4.14 Relative density of the specimens formed by die pressing, slip casting, and pressure filtration. 48 Fig. 4.15 Fracture surface of the specimens formed by die pressing sintered at (a)1350oC, (b)1400oC, (c)1450oC, and (d)1500oC. 51 Fig. 4.16 Thermally etched surface of the specimens formed by die pressing sintered at (a)1350oC, (b)1400oC, (c)1450oC, and (d)1500oC. 52 Fig. 4.17 Some cracks and defects are found on the surface of the sintered specimens formed by die pressing. 53 Fig. 4.18 Fracture surface of the specimens formed by slip casting sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 54 Fig. 4.19 Thermally etched surface of the sintered specimens formed by slip casting sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 55 Fig. 4.20 (a)Second electron image and (b)back scattered electron image of the polished surface of the sintered bulks formed by slip casting. 56 Fig. 4.21 Fracture surface of the specimens formed by pressure filtration sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 57 Fig. 4.22 Thermally etched surface of the sintered specimens formed by pressure filtration sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 58 Fig. 4.23 Average grain size of the specimens formed by die pressing, slip casting, and pressure filtration. 59 Fig. 4.24 In-line transmission of the sintered specimens formed by die pressing. 60 Fig. 4.25 In-line transmission of the sintered specimens formed by slip casting. 61 Fig. 4.26 In-line transmission of the sintered specimens formed by pressure filtration. 61 Fig. 4.27 XRD patterns of the sintered specimens formed by pressure filtration 62 Fig. 4.28 Linear shrinkage of PA, 005E, and 010E during the heating up stage to 1400oC. 63 Fig. 4.29 Fracture surface of the 050E specimens sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 65 Fig. 4.30 Fracture surface of the 001E specimens sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 66 Fig. 4.31 Thermally etched surface of the 005E specimens sintered at (a)1300oC, (b)1350C, and (c)1400C. 67 Fig. 4.32 Thermally etched surface of the 010E specimens sintered at (a)1300oC, (b)1350oC, and (c)1400oC. 68 Fig. 4.33 Fracture surface of the 005E specimens sintered at (a)1300oC, (b)1350oC, and (c)1400oC in the BSE mode. 69 Fig. 4.34 Fracture surface of the 010E specimens sintered at (a)1300oC, (b)1350oC, and (c)1400oC in the BSE mode. 70 Fig. 4.35 The non-uniform precipitates observed on the fracture surface of the 010E specimen sintered at 1400oC. 71 Fig. 4.36 Relative density of PA, 005E, and 010E specimens after sintering. 72 Fig. 4.37 Average grain size of PA, 005E, and 010E specimens after sintering. 73 Fig. 4.38 In -line transmission of the PA, 005E, 010E specimens sintered at 1350oC. 74 Fig. 4.39 In-line transmission of the PA, 005E, 010E specimens sintered at 1400oC. 74 Fig. 4.40 XRD patterns of PA, 005E, and 010E specimen sintered at 1350oC. 75 Fig. 4.41 XRD patterns of PA, 005E, and 010E specimen sintered at 1400oC. 76 Fig. 5.1 The pH value of the alumina suspension with a solid content of 72.6wt% versus various dispersant amounts. 79 Fig. 5.2 The zeta potential value of the alumina suspension versus various pH values. 80 Fig. 5.3 The predicted configuration of the ammonium polyacrylate polymers absorbed on the alumina particles [60]. 80 Fig. 5.4 Relative density of the specimens formed by die pressing, slip casting, and pressure filtration during the heating up stage. 84 Fig. 5.5 AGG and elongated grains (a)in the specimens formed by slip casting then sintered at 1350oC in the present study, and (b)in the specimens doped with 344ppm Ca2+ and sintered at 1400oC in the study by Arzu Altay [70]. 85 Fig. 5.6 Grain size distribution of the specimen formed by slip casting then sintered at 1350°C. 85 Fig. 5.7 Grain size distribution of the specimen formed by slip casting then sintered at 1400°C. 86 Fig. 5.8 (a)SE image and the (b)BSE image of the fracture surface of the 005E specimen sintered at 1450°C. (c)SE image and the (d)BSE image of the fracture surface of the 010E specimen sintered at 1450°C. 88 Fig. 5.9 A summary on relative density and average grain size of pure PCA formed by die pressing, slip casting, and pressure filtration. 90 Fig. 5.10 Second phase precipitates observed (a)in the 010E specimen in the present study, and (b)in the study by K. Drdlíková [46] in his nano-Er2O3 doped PCA specimen. 92 LIST OF TABLES Table 2.1 Some properties of α-Al2O3 [17, 20-23] 5 Table 2.2 A review list of optical PCA by different methods [34-40]. 8 Table 3.1 Information of the dispersant D-305 23 Table 3.2 Notation of the specimens formed by pressure filtration. 31 Table 4.1 EDS analysis of the inclusion (pointed by an arrow) in Fig. 4.19b. 58 Table 4.2 EDS analysis of the precipitates observed in the 010E specimen. 71 | |
| dc.language.iso | en | |
| dc.subject | 製程 | zh_TW |
| dc.subject | 壓濾成形 | zh_TW |
| dc.subject | 注漿成形 | zh_TW |
| dc.subject | 透光陶瓷 | zh_TW |
| dc.subject | 多晶氧化鋁 | zh_TW |
| dc.subject | processing | en |
| dc.subject | pressure filtration | en |
| dc.subject | slip casting | en |
| dc.subject | optical ceramics | en |
| dc.subject | polycrystalline alumina | en |
| dc.title | 以壓濾成形法製備透光多晶氧化鋁 | zh_TW |
| dc.title | Preparation of translucent polycrystalline alumina by a pressure filtration technique | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 106-2 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 黃啟原,施劭儒,劉哲原,許沛衣 | |
| dc.subject.keyword | 多晶氧化鋁,透光陶瓷,製程,注漿成形,壓濾成形, | zh_TW |
| dc.subject.keyword | polycrystalline alumina,optical ceramics,processing,slip casting,pressure filtration, | en |
| dc.relation.page | 104 | |
| dc.identifier.doi | 10.6342/NTU201801948 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2018-08-08 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 材料科學與工程學研究所 | zh_TW |
| dc.date.embargo-lift | 2023-08-10 | - |
| 顯示於系所單位： | 材料科學與工程學系 | |
文件中的檔案：
| 檔案 | 大小 | 格式 | |
|---|---|---|---|
| ntu-107-R05527031-1.pdf 未授權公開取用 | 8.59 MB | Adobe PDF |
系統中的文件，除了特別指名其著作權條款之外，均受到著作權保護，並且保留所有的權利。