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研究生：	陳偉修 Chen, Wei-Hsio
論文名稱：	以Spark Plasma Sintering 製備碳化鎢/氧化鋁奈米複合材料之燒結行為、微結構與材料特性研究 The sintering behavior, microstructure and materials properties of tungsten carbide - alumina nanocomposites fabricated by spark plasma sintering
指導教授：	黃肇瑞 Huang, Jow-Lay
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2015
畢業學年度：	103
語文別：	英文
論文頁數：	126
中文關鍵詞：	噴流床、碳化熱處理、磨耗測試、奈米複合材料
外文關鍵詞：	Spark plasma sintering, spouted bed, carburization, wear test, nanocomposites
相關次數：	點閱：144 下載：6
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在本研究中，藉由Spark plasma sintering 製備WC-Al2O3複合材料對其緻密化行為及微結構及機械性質進行研究。初始材料使用有機金屬化學氣相沉積法結合噴流床製備；其中，W(CO)6被作為前驅物和Al2O3的粉末在噴流床製備合成WC-Al2O3奈米複合粉體。W(CO)6的分解產生非晶氧化鎢並沉積於Al2O3晶粒，在CH4-H2混合氣碳化形成碳化鎢-氧化鋁複合粉末物種。碳化鎢 - 氧化鋁複合體粉末經由SPS在1200到1400°C的溫度進行燒結。在此燒結溫度範圍，SPS燒結的試片包含W、WC和W2C等的第二相，在1350 °C得到純的W2C相。並針對其密度，硬度和電阻率進行研究。

首先，透過金屬有機化學氣相沉積(MOCVD)在噴流床及在CH 4-H2氣氛下於600-900℃下合成奈米碳化鎢顆粒。碳化熱處理主要藉由透過碳原子附著於裂解的非晶氧化鎢的外層，並經持續的碳擴散進入非晶氧化鎢顆粒中，在相轉變過程中，從介穩態的W2C轉變成純的WC相。最初低溫形成的W2C隨著碳化持溫時間的增長及碳化溫度的提高可有效將其轉變為WC相。

其次，藉由添加WC抑制氧化鋁晶粒之成長，進而得到顆粒尺寸300-500奈米的顯微結構來改善WC-Al2O3奈米複合陶瓷的燒結行為和提升其機械性質。WC-Al2O3奈米複合陶瓷在微觀結構上變化，其硬度和斷裂韌性值隨著晶粒尺寸的縮小而有明顯之提升。從顯微結構觀察發現，奈米WC顆粒均勻附著於氧化鋁的晶粒及晶界，進而去抑制氧化鋁基材的晶粒生長。藉由奈米第二相之添加，其破壞模式會從單一相Al2O3的沿晶破壞轉變至WC-Al2O3奈米複合材料的穿晶破壞，進而提升其機械性質。

　　最後，將Spark plasma sintering 製備的WC-Al2O3奈米複合陶瓷探討其磨耗之研究，在室溫環境進行氧化鋁磨球對氧化鋁及WC-Al2O3奈米複合材料磨耗測試。純氧化鋁及WC-Al2O3複合材料對氧化鋁球的主要磨耗行為是塑性變形。而氧化鋁材上裂縫之形成和晶粒拉出在磨損過程會提高其磨耗率。

In this study, the densification behavior of WC-Al2O3 composites prepared via spark plasma sintering (SPS) was investigated. The initial materials were fabricated using a metal-organic chemical vapor deposition process, in which tungsten hexacarbonyl W(CO)6 was used as a precursor and WC-Al2O3 powders were used as the matrix in a spouted chamber. The decomposition of W(CO)6 produced W species that coated the WC-Al2O3 powder and carbonized in CH4-H2 mixing gas to form tungsten carbide-alumina composite powder. The tungsten carbide-alumina composite powder was sintered via SPS in the temperature range of 1200 to 1400 °C. In the above temperature range, secondary phases of W including WC and W2C were found to co-exist in the SPS-treated samples and WC decomposed to form W2C at 1350 °C. The density, hardness, and electrical resistivity of the SPS-treated samples were investigated.
Before synthesis of tungsten carbide-alumina composite powder, nanostructured tungsten carbide particles were successfully synthesized by metal–organic chemical vapor deposition (MOCVD) in a spouted bed followed by carburization in CH4-H2 atmosphere in the temperature range 700–900°C. The carburization process was little bit of complex, which involved the coating of carbon on the outer surface of the decomposed W(CO)6 precursor particles and then followed by carbon diffusion into the particles, leading to formation of nanostructured WC via an intermediate metastable phase W2C. The carbon deficient phase W2C was formed initially at lower carburization temperature and then transformed to stable WC phase by increasing the temperature and holding time.
The materials characteristics of tungsten carbide-alumina composite powder are summarized as follows. The addition of WC improved the sintering process and mechanical properties of WC-Al2O3 matrix by hindering its grain growth. Due to the refined microstructure of composites, the hardness and fracture toughness value were found to be increased with the decrease of the WC-Al2O3 the grain size. The WC-Al2O3 composites show maximum toughness of 6.1 MPa•m1/2 and hardness value of 24 GPa, which are higher than those of monolithic alumina. Microstructure observations indicate that WC nanoparticles are dispersed within the alumina matrix which limits the grain growth of alumina matrix. The fracture mode changes from intergranular in the case of monolithic Al2O3 to transgranular mode for nanocomposites to reinforce their mechanical properties.
Various alumina/tungsten carbide based nanocomposites have been fabricated by spark plasma sintering and their wear properties have been investigated by performing ball-on-disk type wear test at room temperature under ambient environment. The results reveal that the main fracture behavior of the Al2O3/tungsten carbide composites sliding against Al2O3 balls is the plastic deformation. Crack formation and grain pull-out in the wear processes are responsible for enhancing the wear rate.

摘要    	I
Abstract  	III
Acknowledgement	V
Contents  	VII
List of Tables	IX
List of Figures	X
Chapter 1 Introduction	1
1-1 Introduction	1
1-2 Motivation and Objectives	3
Chapter 2 Literature survey	5
2-1 Nanocomposite ceramics	5
2-2 Metal-Organic Chemical Vapor Deposition and Spouted Bed	11
2-2-1 Metal-Organic Chemical Vapor Deposition (MOCVD)	11
2-2-2 Spouted bed	13
2-3 Effect of second phase on the ceramics nanocomposite materials	15
2-3-1 Strengthening mechanisms of ceramic matrix composites	15
2-3-2 Toughening mechanisms of ceramics nanocomposite material	16
2-4 Formation of tungsten carbide via carburized thermal treatment	23
2-5 Spark plasma sintering (SPS)	26
2-6 Wear  	29
Chapter 3 Experimental procedures	34
3-1 Experimental flow chart	34
3-1-1 Pyrolysis of W(CO)6 precursor	36
3-1-2 Preparation of nanocomposite powder	36
3-2 Carburization treatment	39
3-3 Experiment materials	39
3-4 Densification by SPS	42
3-5 Characterization of materials	45
3-5-1 Thermo gravimetric analysis	45
3-5-2 Phase identification by X-ray diffraction	45
3-5-3 Microstructural observation	46
3-5-4 X-ray photoelectron Spectroscopy	46
3-5-5 Density measurement	46
3-5-6 Mechanical Properties	47
3-5-7 Electrical property	48
3-5-8 Nanoindentation	48
3-5-9 Sliding wear test	49
Chapter 4 Characterization of powder	52
4-1 Preparation and characterization of decomposed precursors	52
4-1-1 Analysis of W(CO)6 precursor	52
4-1-2 The microstructure of decomposed W(CO)6	55
4-1-3 Carburization of decomposed W(CO)6 powder	57
4-2 Preparation and characterization of the nanocomposite materials	67
4-2-1 The microstructure of the nanocomposite materials	67
4-2-2 Carburization and characterization of the nanocomposite materials	70
Chapter 5 Sintering behavior and mechanical properties of tungsten carbide–alumina composites	74
5-1 The effect of sintering temperature on the nanocomposite	74
5-1-1 Characterization	74
5-1-2 Property of SPS-treated composites	80
5-2 Effect of the carburized time on composites	86
5-2-1 Characterization	86
5-2-2 Property of SPS-treated composites	89
5-2-3 Toughening mechanism of SPS-treated composites	93
5-3 The effects of WC contents on the characteristic of WC-Al2O3 composites	95
5-3-1 Sintering behavior	95
5-3-2 Microstructure and mechanical properties	97
5-3-3 Nanoindentation	101
Chapter 6 Wear behavior of WC/Al2O3 composite	107
6-1 Characterization	107
6-2 Wear test	109
Chapter 7 Conclusions	113
References	114
List of Publications	124
                                    

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