製作連續規則斷面的產品，通常使用擠製成形，而氧化鋯陶瓷為硬脆材料，必須以粉末冶金的方法，使陶瓷粉末成為具有可塑性的膏狀材料（Paste Material），以利擠製成形（Extrusion）。擠製後的棒狀生胚再經燒結獲得成品。本研究的目的為找出擠製氧化鋯（Zirconia）陶瓷材料之最佳化參數及各參數設定對品質之影響程度，因此使用田口法（Taguchi Methods）設計參數及實驗，將參數選定為形成膏狀材料的方法、擠型比、擠製速度、燒結後持溫，品質特性選定為抗折強度、硬度、孔隙率及晶粒尺寸，並使用變異數分析（analysis of variance, ANOVA），計算出各參數的貢獻度（重要性），進一步找出實驗最佳參數，預測最佳值。結果顯示形成膏狀材料的方法、擠型比、擠製速度、燒結後持溫，此四個參數中以形成膏狀材料的方法對本研究之品質影響程度最大；在形成膏狀材料的方法為主體粉末(3YSZ)+12 wt%乙醇+8 wt%甘油、擠型比為16:1、擠製速度15 mm/min、在1450℃燒結兩小時後爐冷為本實驗之最佳參數組合，其可產生平均約1190 MPa抗折強度、1322 Hv硬度、1.6547 vol%孔隙率及307 nm晶粒尺寸之氧化鋯擠製棒材。

The extrusion processes are commonly applied for the parts with continuously constant cross-sections. The zirconia has high hardness to be manufacture by powder metallurgy. The paste materials of zirconia are prepared and then extruded followed by sintering to be rod-type of parts for tooling. This study determines the experiment parameters by Taguchi analysis. The four parameters including formula of paste material, extrusion ratio, extrusion speed and sintering process are choosed using analysis of variance (ANOVA), which are used to experimentally extrude the zirconia. The properties of the extrudate such as porosity、 grain size、 hardness and transverse rupture strength (TRS) are measured and compared with the ANOVA. The results indicate that the formula of paste materials plays the most important parameter on properties. The conditions including paste materials comprised of 12 wt% alcohol, 8 wt% glycerin and balance zirconia、 16:1 of extrusion ratio、 15 mm/min of extrusion speed and 2 hours sintering at 1450 ℃ followed by furnace cooling are the optimal options, by which the properties such as 1.6547 vol% of porosity, average 307 nm of grain size, average 1322 Hv of hardness and average 1190 MPa of TRS are obtained.

目錄 I
表目錄 III
圖目錄 IV
第一章 緒論 1
1.1 研究目的與動機 1
第二章 基礎的理論與文獻探討 2
2.1 氧化鋯材料 2
2.2 膏狀材料擠製理論 7
2.3 田口實驗計劃法 11
2.3.1 品質損失函數 11
2.3.2 品質特性的訂定 12
2.3.3 訊號雜訊比 12
2.3.4 直交表 13
2.3.5 變異數分析 13
2.3.6 確認 14
第三章 實驗架構 15
3.1 實驗材料、模具與設備 15
3.1.1 粉末材料方面 15
3.1.2 擠製模具方面 15
3.1.3 擠形製程儀器設備方面 16
3.1.4 燒結設備 17
3.2 實驗的計畫與流程 18
3.2.1 擠型過程 19
3.3 實驗的量測與分析 20
3.3.1 抗折強度量測 20
3.3.2 密度量測 21
3.3.3 硬度量測 22
3.3.4 顯微組織觀察 22
3.3.5 相分析 23
第四章 結果與討論 24
4.1 田口實驗計劃法 24
4.1.1 問題解析 24
4.1.2 決定品質特性 25
4.1.3 列出影響品質特性的因子 25
4.1.4 決定控制因子及變動水準 26
4.1.5 建構直交表 29
4.1.6 執行實驗 30
4.1.7 實驗數據之量測 31
4.1.8 因子反應分析 39
4.2 參數分析及擠型最佳化 40
4.3 確認 45
第五章 結論 48
參考文獻 49
附錄A 51
附錄B 52

[1] D. J. Garvie, R. H. J. Hannink, and M. V. Swain, 1989, “Transformation Toughening of Ceramics”, CRC Press.
[2] R. C. Garive, R. H. Hannink and R. T. Pascoe, 1975, “Ceramic Steel”, Nature（London）, 258（5537）, pp. 703-704.
[3] B. Basu, 2005, “Toughening of yttria-stabilised tetragonal zirconia ceramics”, International Materials Review, vol. 50, no.4.
[4] J. S. Reed and T. J. Martin, 1960, “Mechanics of Extrusion”, Science of Whitewares, The American Ceramic Society, Ohio, pp 157-198.
[5] J. J. Benbow, T. A. Lawson, E. W. Oxley and J. Bridgwater, 1989, “Prediction of paste extrusion pressure”, Am. Ceram. Soc. Bull. pp. 821-824.
[6] Z. Chen, K. Ikeda, T. Murakami, T. Takeda and J.-X. Xie, 2003, “Fabrication of composite pipes by multi-billet extrusion technique”, Journal of Materials Processing Technology, vol. 137, pp. 10-16.
[7] E. H. Kisi, C. J. Howard, 1998. “Crystal Structure of Zirconia Phases and their Inter-relation”, Zirconia Engineering Ceramics: old challenges-new ideas, Trans Tech Publications.
[8] 史宗淮，2002， “奈米氧化鋯微粒製程與精密陶瓷之應用” ，工程， pp. 30-38。
[9] Raymond A. Cutler, James R. Reynolds, and Aaron Jones, 1992,“Sintering and Characterization of Polycrystalline Monoclinic, Tetragonal, and Cubic Zirconia”, Journal of the American Ceramic Society, vol. 75 [8], pp. 2173.
[10] E. Barbier and F. Thevenot, 1991, “Titanium Carbontride-Zirconia Composites: Formation and Characterization”, Journal of the European Ceramic Society, vol. 8, pp. 263.
[11] 龔淑怡，2004，“氧化鋯陶瓷粉末之擠製研究”，國立高雄應用科技大學模具系所碩士論文。
[12] John Benbow and John Bridgwater, 1993, Paste Flow and Extrusion, Clarend on press, Oxford.
[13] 吳復強，1992，“田口品質工程”，全威，台北。
[14] O. Kempthome, 1979, “The Design and Analysis of Experiments”, Robert E. Krieger Publishing Co., NewYork.
[15] R. L. Plackett and K. P. Burman, “The Design of Optimal Multifactorial Experiments”, Biometrika, vol. 33, pp. 305-325.
[16] S. Addelman, 1962, “Orthogonal Main Effect Plans for Asymmetrical Factorial Experiments”, Technomitrics, vol.4 pp. 21-46.
[17] D. Raghavarao, 1971, “Construction of Combinatorial Problems in Design Experiments”, John Wiley and Sons, New York.
[18] E. Seiden, 1954, “On the Problem of Construction of Orthogonal Arrays”, Annals of Mathematical Statistics, Vol. 25, pp. 151-156.
[19] G. Taguchi（English translation）, 1987, System of Experimental Design, Edited by C. Don, UNIPUB/Kraus International Publications, New York, Vol. 1 and 2.
[20] 黎中正 編譯，1993，“穩健設計之品質工程”， 台北圖書有限公司，台北。
[21] 李輝煌，2008，“田口方法-品質設計的原理與實務”，高立圖書有限公司。
[22] 施博文，2006，“真空擠製氧化鋯陶瓷粉末擠製參數對機械性質之影響”，國立高雄應用科技大學模具系所碩士論文。
[23] J. J. Benbow, J. Bridgwater, 1993, “Paste flow and extrusion”, Clarendon Press, Oxford.
[24] J. J. Benbow, E. W. Oxley and J. Bridgwater, 1987, “The extrusion mechanics of paste-The influence of paste formulation on extrusion parameters”, Chem. Engineering Science, vol. 42, no.9, pp. 2151-2162.
[25] Z. Toutou, N. Roussel and C. Lanos, 2005, “The squeezing test: a tool to identify firm cement-based material’s rheological behaviour and evaluate their extrusion ability”, Cement and Conerete Research, vol. 35, pp. 1891-1899.
[26] R. N. Das, C. D. Madhusoodana and K. Okada, 2002, “Rheological studies on cordierite honeycomb extrusion”, Journal of the European Ceramic Society, vol. 22, pp. 2893-2900.
[27] Annette Therese Jocelyn Domanti, 1998, “Surface Fracture in Paste Extrusion”, PhD Thesis, University of Cambridge, U. K.
[28] X. H. Wang, P. L. Chen and I. W. Chen, 2006, “Two-step sintering of ceramics with constant grain-size, I. Y2O3”, J. Am. Ceram. Sac. , 89[2], pp. 431-437.
[29] Y. I. Lee, Y. W. Kim and M. Mitomo, 2004, “Effect of processing on densification of nanostructured SiC ceramics fabricated by two-step sintering”, Journal of Materials Science, vol. 39, pp. 3801-3803.
[30] X. H. Wang, X. Y. Deng, H. Zhou, L. T. Li and I. W. Chen, 2007, “Bulk dense nanocrystalline BaTiO3 ceramics prepared by novel pressureless two-step sintering method”, J Electroceram.