博碩士論文 87321011 詳細資訊




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姓名 廖國宏(Kuo-Hong Liao)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 矽粉對二氧化矽碳熱還原氮化反應影響之研究
(The Influence of silicon on the Carbothermal Reduction and Nitriding of Silica)
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摘要(中) 本研究為以矽粉為添加劑,在氮氣環境下進行二氧化矽的碳熱還原反應,探討矽粉添加劑對反應產物的形態與反應速率等之影響,並深入研究矽粉添加劑於反應中所扮演之角色。研究中使用直立式管狀高溫爐,由反應前後之重量變化求得二氧化矽之轉化率,以探討各項操作變數對反應之影響。
本文主要探討的因素包括:氮氣流率、矽粉添加量、C/SiO2莫耳數比、樣品載量及反應溫度等。研究中並做各種物性分析(感應耦合電漿質譜分析儀、比表面積測定儀、X-射線繞射儀、低真空掃描式電子顯微鏡等)來提供各項實驗結果之佐證。
實驗結果顯示,增大氮氣流率可增加二氧化矽之轉化率,當氣體流率大於500 ml/min時,則影響並不明顯;添加矽粉可增加二氧化矽之轉化率;過量的碳可提高二氧化矽的轉化率,當C/SiO2莫耳數比大於5時,影響漸減;而減小反應物載量亦可增加二氧化矽之轉化率;升高反應溫度則可明顯的促進反應速率。添加矽粉氮化反應的產物為碳化矽,其型態主要為纖維狀的結晶。推測矽粉添加造成一氧化矽的大量生成與一氧化矽是經由矽粉還原二氧化矽而來,是碳化矽成長的重要機制。
摘要(英) The carbothermal reduction and nitridation of silicon dioxide with silicon powder addition was investigated by weight gain measurement. The reaction were carried out in a vertical reaction tube heated by a tubular furnace. In this study, the operating variables have been discussed included: nitrogen flow rate, amount of silicon powder added in the reactant, silicon dioxide/carbon molar ratio, sample weight, and reaction temperature. The analysis of this experiment is conducted by X-ray diffraction (XRD), scanning electron microscope (SEM), BET surface area, and inductively coupled plasma-mass spectrometer (ICP-MS).
The experimental results indicated that the conversion of silicon dioxide is increased with an increasing nitrogen flow rate and the effect is not appreciable when the flow rate exceeds 500ml/min. The conversion of silicon dioxide is increased with an increasing amount of silicon powder added in the reactant. An excess of carbon powder and decrease of the sample weight are required to promote the conversion, however, the effect is not appreciable when the molar ratio is above 5 and sample weight is below 0.3g. Moreover, the reaction rate and the conversion of silicon dioxide is significantly increased with higher reaction temperature. The reaction product is fibrous shape β-SiC with silicon powder addition. We conjectured that the large formation of gaseous SiO is an important way for β-SiC growth.
關鍵字(中) ★ 添加劑
★ 氮化反應
★ 碳熱還原
★ 二氧化矽
★ 碳化矽
★ 氮化矽
關鍵字(英) ★ carbothermal reduction
★ silicon dioxide
★ silicon carbide
★ silicon nitride
★ nitridation
★ additive
論文目次 中文摘要I
英文摘要II
目錄III
圖索引V
表索引VIII
符號說明IX
第一章 緒論1
第二章 文獻回顧9
2.1 氮化矽之型態結構10
2.2 二氧化矽之碳熱還原反應13
第三章 理論背景21
3.1 氮化矽的生成機構21
3.2 矽粉添加劑造成反應機構的變化27
3.3 動力學上的分析28
3.4 二氧化矽轉化率的計算31
第四章 實驗部份35
4.1 藥品及氣體35
4.2 儀器設備35
4.3 試樣之前處理38
4.4 氮化反應系統39
4.5 反應物的金屬成分分析43
4.6 試樣之物性分析44
4.7 實驗流程概要和操作變數50
第五章 結果與討論52
5.1 試樣物性之分析結果52
5.2 二氧化矽之還原條件探討65
5.3 反應機構之探討75
第六章 結論79
參考文獻81
附錄 實驗數據
參考文獻 1. Badrak. S. A., T. S. Bartnitskaya, and I. M. Baryshevskay, et al., “Thermodynamic Calculations for the Assessment of Possible Ways of Formation of Silicon Nitride”, Porohk. Metall., No 9, 66(1981).
2. Blumenthal J. I., M. J. Santy and F. A. Burns, AIAA J., 4, 1053(1966).
3. Cho Y. M. and J. A. Charles, “Synthesis of Nitrogen Ceramic Powders by Carbothermal Reduction and Nitridation Part 1 Silicon Nitride “, Mater. Sci. and Tech., Vol.7, 289(1991).
4. Durham B. G., Marlyn J. Murtha, and George Burnet, “Si3N4 by the Carbothermal Ammonolysis of Silica ”, Adv. Ceram. Mater, 3(1), 45(1988).
5. Durham S. J. P., K. Shanker, and R. A. L. Drew, “Carbothermal Synthesis of Silicon Nitride: Effect of Reaction Conditions “, J. Am. Ceram. Soc., 74(1), 31 (1991).
6. Durham S. J. P., K. Shanker, and R. A. L. Drew, “Silicon Nitride Particle Formation During Carbothermal Reduction “, P.313 in Ceramic Powder Processing Science. Edited by H. hausner, G. Messing, and S. Hirano. Deutsche Keramische Gesellschaft, Koln, FRG, (1989).
7. Durham S. J. P., K. Shanker, and R. A. L. Drew, “ Thermochemistry of the Si-O-N-C System with Relation to the Formation of Silicon Nitride “, Can. Metall. Q., 30(1), 39-43(1991).
8. Ekelund, M. and B. Forslund, “Carbothermal Preparation of Silicon Nitride: Influence of Starting Material and Synthesis Parameters “, J. Am. Ceram. Soc., 75(3), 532-539(1991).
9. Ekelund, M. and B. Forslund, “Reactions whthin Quartz-Carbon Mixtures in a Nitrogen Atmosphere “, J. Eur. Ceram. Soc., 9(2), 107-119, (1992).
10. Fiqusch V. and T. Licko, “Synthesis of Silicon Nitride Powder by Carbothermal Nitriding of Silica “, P.157 in High Tech Ceramics. Edited by P.Vincenzini. Elsevier, Amsterdam, The Netherlands, (1987).
11. Han W., S. Fan, Q. Lee, B. Gu, X. Zhang, and D. Yu, “Synthesis of Silicon Nitride Nanorods Using Carbon Nanotube as a Template”,Appl. Phys. Lett.,71(16),2271-2273(1998)
12. Hendry A. and K. H. Jack, In Special Ceramics (edited by P. Popper). P.199 Br. Cer. Res. Assoc., Stoke on Trent (1975).
13. Hirosaki N., Y. Akimune, and M. Mitomo, “Effect of Grain-Growth of Beta-Silicon Nitride on strength, Weibull Modulus, and Fraacture —Toughness“,J. Am. Ceram. Soc.,76(7),1892(1993).
14. Inoue H., K. Komeya, and A. Tsuge, ”Synthesis of Silicon Nitride Powder from Silica Reduction “, Comm. of the Amer. Ceram. Soc., December, C-205 (1982).
15. Jack K. H., “In Progress of Nitrogen Ceramic “, Edited by F. L. Riely. Martins Nijhoff Publishers, Boston, P.465 (1983).
16. Koc R., and S. Kaza, ”Synthesis of α-Si3N4 from Carbo Coated Silica by Carbothermal Reduction and Nitridation”,J. Eur. Ceram. Soc.,18,1471-1477(1998)
17. Komeya K., and H. Inoue, “Synthesis of the
指導教授 張奉文(Feg-Wen Chang) 審核日期 2000-7-7
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