以微波及傳統水煮聚合四種不同品牌（QC-20，Pladent-20，Optilon-399，Hygenic）之假牙樹脂。將糰狀態樹脂以纖維補強塑膠包埋盒經過標準程序包埋後，置於微波爐內，以熱電偶分別記錄尺寸為65 mm’15 mm’10 mm的樹脂在80、160及240瓦受微波照射時溫度對時間之變化。微波聚合利用相同之設備，條件為80、160、240及560瓦分別照射15、10、7及2分鐘，完成後再翻面置於560瓦下照射2分鐘。水煮試件則是以金屬包埋盒包埋後置於70℃熱水煮聚9小時。每組條件皆聚合10塊試件。測試每一塊試件之表面硬度、空孔分佈、三點撓曲性質以及溶解度。以160 KV穿透式電子顯微鏡（TEM）觀察Optilon-399之形態。試片經過超薄切片機切片後，以2 %鋨酸（Osmium tetroxide）染色2天。結果顯示樹脂並非等速聚合，不同樹脂在同一時間有相差約30℃的現象產生。除了Paladent-20之外，表面硬度值變化不大。空孔含量隨著瓦數的增加有上升之趨勢。添加韌性成分之Optilon-399樹脂，採用水煮法之撓曲強度高出微波試件約20MPa，但不同瓦數間之強度相似。Optilon-399在聚合後會有相分離產生，分散相主要是以兩種形式存在，一為含富橡膠相的區域內包含微小PMMA相之區域，其直徑在0.18 mm至0.67 mm之間，另一為含富橡膠相之球形區域，直徑約為0.1 mm。聚合時間長短決定分散相之平均直徑及數量。水煮法試片具有最大之平均直徑（0.395±0.068 mm）。隨著瓦數之增加，直徑有縮小之趨勢。單一試件中不同位置其內部形態亦不同，80瓦時分散相面積大小所對應之圓形直徑相差0.03 mm，而560瓦則相差0.05 mm，顯示瓦數愈高，分散相之面積差異愈明顯。

Four denture base materials of poly(methyl methacrylate) (QC-20, Pladent-20, Hygenic, and Optilon-399) were prepared by convention water bath and microwave-energy cured methods. While the resin was in the dough stage, it was packed into two molds (65 mm ’15 mm ’10 mm) in the fiber reinforced plastic flask. The variation of temperature with time was recorded by two thermocouples during the microwave heating at 80, 160, and 240 watts, respectively. Microwave polymerization was carried out in the same equipment. The microwave flask containing the same size of resin blocks were processed at 80, 160, 240, and 560 watts for 15, 10, 7, and 2 min, separately. Then each flask was turned over, and cured an additional 2 min at 560 watts. In the case of water-bath method, the resin in the dough stage was packed in the Brass flask, and then cured at 70℃ for 9 hours. Ten specimens were prepared for each condition studied. The surface hardness, porosity, flexural properties and solubility of both process conditions were evaluated. The samples were sectioned by microtome and stained 2 % Osmiun tetroxide, then the morphology of Optilon-399 was observed by using TEM (Transmission electron microscopy) at 160 KV. The result indicate that the flexural strength for Optilon-399 specimens prepared by water-bath method was 20 MPa higher than that prepared in microwave oven, however, there were no obvious difference between the samples cured at different power. Phase separation in two different sizes was observed in all of the Optilon-399 specimens. The larger domain was with 0.18 mm~0.67 mm diameter has dispersed rubber phase surrounded by a rubber periphery. The smaller domain with 0.1 mm diameter is rich with rubber phase. The size and distribution of the larger domain were correlated with the microwave power and curing time. The sample cured by water-bath has the largest average domain diameter (0.395±0.068 mm). In the specimens prepared by microwave method, the domain size decreased with increasing power. In additions, the domain size varied across the specimen. The size difference between the largest and the smallest domain for specimens cured at 80W was 0.03 mm, and that for specimens cured at 560W was 0.05 mm. This indicated that the larger the power watt was, the higher the morphology difference was.

目錄 I
表目錄 V
圖目錄 VII
中文摘要 X
英文摘要 XI

第一章 緒論 1
第二章 基本理論 2
2.1 聚甲基丙烯酸甲酯 2
2.2 聚甲基丙烯酸甲酯型假牙樹脂之主要成份 3
2.3 義齒基底製作過程 5
2.4 微波及其特性 8
2.5 微波聚合 11
第三章 文獻回顧 16
3.1 微波聚合的發展 16
3.2 微波聚合樹脂之物理性質 18
3.2.1 橫斷強度 19
3.2.2 表面硬度 19
3.2.3 多孔性 20
3.2.4 貼合性 23
3.2.5 殘餘單體 24
第四章 決定微波時間及聚合試件 26
4.1 前言 26
4.2 實驗材料 26
4.3 實驗儀器 26
4.4 決定微波時間 27
4.6 結論 36
第五章 基本性質與機械性質實驗 45
5.1 前言 45
5.2 實驗材料 45
5.3 實驗儀器 46
5.4 實驗流程 46
5.5 實驗方法 47
5.5.1 超音波空孔掃瞄 47
5.5.2 硬度測試 48
5.5.3 撓曲性質測試 50
5.5.4 溶解度 51
5.6 結果與討論 52
5.6.1 溶解度 52
5.6.2 硬度 52
5.6.3 空孔數 54
5.6.4 撓曲性質 56
5.7 結論 58
第六章 形態觀察 66
6.1 前言 66
6.2文獻回顧 67
6.4 實驗材料 70
6.5 實驗儀器 70
6.6 實驗流程圖 70
6.7 實驗部分 70
6.7.1 試件編號 71
6.7.2 TEM試片製作 71
6.8 實驗結果 73
6.8.1 破斷面形態觀察 73
6.8.2 不同位置形態觀察 76
6.9 討論 77
6.9.1 破斷面形態觀察 77
6.9.2 不同位置形態觀察 79
6.10 結論 82
第七章 空孔多寡與韌性區域大小對撓曲性質之影響 103
7.1 前言 103
7.2 影響樹脂撓曲性質之主要因素 103
7.3 結論 106
第八章 結論 109
第九章 參考文獻 111


表目錄
頁碼
Table 1 Principal ingredients of denture base powder and liquid. 13
Table 2 Materials used in this study. 37
Table 3 Properties and structure of denture base compositions. 38
Table 4 Curing cycle employed in the study. 39
Table 5 The solubility of denture base resins. 59
Table 6 The hardness of denture base resins. 59
Table 7 The porosity of denture base resins. 60
Table 8 Flexural strength of four denture base resins cured by microwave and water-bath. The ratio of distance between supports and resin width was 4; the crosshead speed was 1.25mm/min 60
Table 9 Flexural displacement of four denture base resins cured by microwave and water-bath. The ratio of distance between supports and resin width was 4; the crosshead speed was 1.25mm/min 61
Table 10 Flexural modulus of four denture base resins curing by microwave and water-bath. The ratio of distance between supports and resin width was 4; the crosshead speed was 1.25mm/min 61
Table 11 Specific functional groups, examples and stains. 83
Table 12 The size, distribution, and percentage area of "R" domain in specimens cured by different conditions. 84
Table 13 Average diameter and standard deviation of "R" domains at the center position of the specimens cured by (a) water-bath method, and microwave output power at (b) 80 W, (c) 160 W, (d) 240 W, (e) 560 W, respectively. 85


圖目錄
頁碼
Fig 1 The glycol dimethacrylate produces a bridging effect between growing polymer chains. 14
Fig. 2 A diagram of the rheology stages from mixing of the powdered polymer and liquid monomer to setting. 15
Fig. 3 Schematic of fiber-reinforced flasks for microwave processing.. 39
Fig. 4 Specimen temperature versus time for microwave power at 80 W. 40
Fig. 5 Specimen temperature versus time for microwave power at 160 W. 41
Fig. 6 Specimen temperature versus time for microwave power at 240 W. 42
Fig. 7 Decomposition of benzoyl peroxide by heat. 43
Fig. 8 Free radical react with monomer. 43
Fig. 9 Optilon-399 specimen temperature versus time for microwave power at 80 W, 160 W, 240 W. 44
Fig. 10 Schematic plot of flow chart. 62
Fig. 11 Schematic diagram of a C-Scan test. 63
Fig. 12 Surface hardness versus loading time. 63
Fig. 13 Schematic diagram of a three-point bending. 64
Fig. 14 C-Scan pictures of resins. 65
Fig. 15 A rubber particle exposed in the fracture surface of rubber toughened denture base resin. 87
Fig. 16 Ultrathin section of the rubber toughened denture base resin stained with Osmium Tetroxide. 87
Fig. 17 Flow chart of TEM experiment. 88
Fig. 18 Schematic of TEM specimen preparation. 89
Fig. 19 Schematic of (a) staining method, (b) the method of washing grids after staining 90
Fig. 20 TEM morphology of Optilon-399 cured by water-bath without staining. 91
Fig. 21 TEM morphology of Optilon-399 cured by water-bath and stained with 2 % Osmium Tetroxide. 92
Fig. 22 TEM morphology of Optilon-399 cured at 80W and stained with 2 % Osmium Tetroxide. 93
Fig. 23 TEM morphology of Optilon-399 cured at 160W and stained with 2 % Osmium Tetroxide. 94
Fig. 24 TEM morphology of Optilon-399 cured at 240W and stained with 2 % Osmium Tetroxide. 95
Fig. 25 TEM morphology of Optilon-399 cured at 560W and stained with 2 % Osmium Tetroxide. 96
Fig. 26 TEM morphology of Optilon-399 cured at 560 W and stained with 2 % OsO4. The formation of "P" domain from "R" domain are imagined to go through A, B,…, F are showed in (a) (b) (c) (d), respectively 97
Fig. 27 The distribution of "R" domain in specimens cured by water-bath and microwave methods. 99
Fig. 28 The distribution of "R" domain in specimens cured by microwave at power of 80, 160, 240, 240 and 560 W, respectively.. 99
Fig. 29 The average diameter of "R" domain in 10 positions. (a)560W (b)80W. 100
Fig. 30 TEM morphology of Optilon-399 cured at 80W and stained with 2 % Osmium Tetroxide. Position (a) 6, and (b) 2.. 101
Fig. 31 TEM morphology of Optilon-399 cured at 560W and stained with 2 % Osmium Tetroxide. Position (a) 8, and (b) 3. 102
Fig. 32 Model of crack propagation in a rubber modified resin. 107
Fig. 33 The domain size, flexural properties, and the porosity for specimens cured by water-bath and microwave methods. 108

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