臺灣博碩士論文加值系統

本研究使用雙螺桿押出機以熔融混練法製備聚己二酸丁二醇酯-共-對苯二甲酸丁二醇酯(PBAT)/聚羥基丁酯戊酯(PHBV)摻合體為基材，添加不同尺寸之微米級纖維素(UFC100、PH105)及紅麻纖維(Kenaf fiber)作為補強材之複合材料，探討兩種纖維素或未改質/改質紅麻纖維對摻合體相形態之影響，並量測複合材熔融/結晶行為、熱穩定性、機械性質、流變性質及吸水性質。藉由SEM及FTIR分析發現，紅麻纖維經鹼改質能去除纖維表面的雜質，矽烷改質可增加紅麻纖維與基材間的界面接合力。SEM與POM分析發現，PBAT/PHBV以重量比例為70:30之摻合體為部分相容系統，PBAT為連續相，PHBV為分散相；添加紅麻纖維或纖維素皆有被拔出(pulled out)及界面空隙產生的現象。TGA分析發現，加入紅麻纖維或纖維素有助於熱穩定性提升。DSC結果發現，添加紅麻纖維或纖維素皆有助於誘導摻合體中PHBV異質成核結晶，卻抑制PBAT結晶。DMA分析發現，隨纖維素或紅麻纖維的含量提升，樣品儲存模數隨之提升，摻合體僅發現一個玻璃轉移溫度(Tg)，可歸因其為部分相容系統，另一相Tg不易觀察到。在機械性質量測方面，加入纖維素或紅麻纖維皆有助提升複合材料的模數及強度，但卻降低斷裂延伸率。流變性質分析發現，隨著纖維素或紅麻纖維含量增加，複合材料之複黏度與儲存模數皆提升。吸水性質分析發現，添加具有親水性之紅麻纖維或纖維素皆會提升複合材料的吸水率，T7V3H30提升最佳顯著。

In this study, poly (butylene adipate-co-terephthalate) (PBAT)/Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) blend-based composites with different sizes of cellulose (PH105, UFC100) and kenaf fiber as fillers were prepared through melt mixing technique in a co-rotating twin-screw extruder. To investigate the effects of two cellulose or untreated/treated kenaf fibers within the polymer matrix on the morphology, the melting/crystallization behavior, thermal stability, mechanical properties, rheological properties and water absorption properties of the composites were discussed. SEM and FTIR analysis showed that impurities on the surface of the fiber were removed after alkali treatment, and alkali-silane treatment can improve interfacial adhesion between kenaf fiber and matrix. SEM and POM analysis showed that the blend of PBAT/PHBV with a weight ratio of 70:30 was a partial compatibility system, PBAT was the continuous phase, PHBV was the dispersed phase, and loading of kenaf fiber or cellulose was pulled out and the phenomenon of interface voids. TGA results showed that the thermal stability of the prepared composites was slightly improved. DSC results showed that fillers helped to induce heterogeneous nucleation crystallization of PHBV in the blend, but inhibited PBAT crystallization. DMA analysis showed that the content of cellulose or kenaf fiber increased, the composites storage modulus increased. Rheological properties analysis showed that the complex viscosity and storage modulus of the composite increased. The results of water absorption showed that the addition of hydrophilic fibers increased the water absorption of the composites, and T7V3H30 improved the most significant.

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摘要 ⅲ
Abstract ⅳ
目錄 ⅴ
圖目錄 ⅷ
表目錄 ⅻ
第一章 緒論 1
第二章 文獻回顧 3
2.1聚己二酸丁二醇酯-共-對苯二甲酸丁二醇酯 (PBAT) 3
2.2聚羥基丁酯戊酯 (PHBV) 4
2.3天然纖維 (Natural fiber) 5
2.4纖維素 (Cellulose) 9
2.5 PBAT/PHBV 摻合體複合材料 10
2.6 PBAT/PHBV/天然纖維摻合體複合材料 11
第三章 實驗 14
3.1 材料 14
3.2 儀器設備 15
3.3樣品製備 18
3.3.1 流程圖 18
3.3.2 未改質纖維之複合材料 19
3.3.3 鹼改質纖維之複合材料 19
3.3.4 鹼-矽烷改質纖維之複合材料 20
3.3.5 纖維素之複合材料 20
3.3.6 射出試片 21
3.4 性質分析 22
3.4.1 傅里葉轉換紅外光譜儀 (FTIR) 22
3.4.2 掃描式電子顯微鏡 (SEM) 22
3.4.3 場發式掃描電子顯微鏡 (FE-SEM) 22
3.4.4 光學顯微鏡 (LM) 22
3.4.5 微示差掃描熱卡計 (DSC) 23
3.4.6 熱重損失分析儀 (TGA) 23
3.4.7 萬能拉力試驗機 (Universal Tensile Machine) 23
3.4.8 耐衝擊試驗機 (Impact Test Machine) 23
3.4.9 動態機械分析儀 (DMA) 23
3.4.10 流變儀 (Rheometer) 23
3.4.11 吸水性 (Water absorption) 24
第四章 結果與討論 25
4.1 紅麻纖維改質鑑定 25
4.1.1 掃描式電子顯微鏡 25
4.1.2 傅里葉轉換紅外光譜分析 27
4.1.3 熱重分析 29
4.2 纖維素 32
4.2.1 掃描式電子顯微鏡 32
4.2.2 熱重分析 34
4.3 摻合體/複合材料之相形態 36
4.3.1 掃描式電子顯微鏡 36
4.3.2 光學顯微鏡 44
4.4 熱性質 53
4.4.1 熱穩定性 53
4.4.2 結晶行為 56
4.4.3 熔融行為 60
4.5 機械性質 65
4.5.1 拉伸性質(Tensile properties) 65
4.5.2 彎曲性質(Flexural properties) 69
4.5.3 衝擊性質(Impact property) 72
4.5.4 動態機械性質 75
4.6 流變性質 79
4.7 吸水性質 82
第五章 結論 84
參考文獻 86

圖目錄
Fig. 2-1 Chemical structure of PBAT. - 3 -
Fig. 2-2 Chemical structure of PHBV. - 4 -
Fig. 2-3-1 Classification of natural and synthetic fibres. - 5 -
Fig. 2-3-2 Life cycle of bio-composites. - 6 -
Fig. 2-3-3 Chemical structure of silane coupling agent. - 8 -
Fig. 2-3-4 Reaction between pineapple leaf fibers and γ-aminopropyl trimethoxy silane. - 8 -
Fig. 2-4 Chemical structure of cellulose. - 9 -
Fig. 4-1-1 SEM micrographs of KF：(a) untreatment (UKF), (b) alkali treatment (AKF) and (c) alkali-silane treatment (ASKF) at 1000x, (d) UKF, (e) AKF and (f) ASKF at 3000x. - 26 -
Fig. 4-1-2 FTIR spectra of UKF, AKF and ASKF. - 28 -
Fig. 4-1-3 FTIR spectra of UKF, AKF and ASKF from 900 to 1800 cm-1. - 28 -
Fig. 4-1-4 (a) TGA and (b) DTG curves of UKF, AKF and ASKF. - 30 -
Fig. 4-2-1 SEM micrographs of cellulose：(a) UFC100 (b) PH105 at 1000x. - 33 -
Fig. 4-2-2 SEM micrographs (50x) of KF. (marked with length and width) - 33 -
Fig. 4-2-3 (a) TGA and (b) DTG curves of UFC100 and PH105. - 35 -
Fig. 4-3-1 SEM micrographs of：(a) PBAT and (b) PHBV at 500x, (c) PBAT and (d) PHBV at 1000x, (e) PBAT and (f) PHBV at 3000x - 38 -
Fig. 4-3-2 SEM micrographs of PBAT at different magnification：(a) 500x, (b) 1000x and (c) 3000x. - 39 -
Fig. 4-3-3 FE-SEM micrograph of PBAT at 20000x. - 39 -
Fig. 4-3-4 SEM micrographs of：(a) T7V3C10, (b) T7V3C30 at 500x, (c) T7V3C10, (d) T7V3C30 at 1000x, (e) T7V3C10, (f) T7V3C30 at 3000x. (Red circle for void, yellow arrow for cellulose ) - 40 -
Fig. 4-3-5 SEM micrographs of：(a) T7V3H10, (b) T7V3H30 at 500x, (c) T7V3H10, (d) T7V3H30 at 1000x, (e) T7V3H10, (f) T7V3H30 at 3000x. (Red circle for void, yellow arrow for cellulose ) - 41 -
Fig. 4-3-6 SEM micrographs of：(a) T7V3UK10, (b) T7V3UK30 at 100x, (c) T7V3UK10, (d) T7V3UK30 at 500x. (Red circle for void, yellow arrow for fiber ) - 42 -
Fig. 4-3-7 SEM micrographs of：(a) T7V3AK30, (b) T7V3ASK30 at 500x, (c) T7V3AK30, (d) T7V3ASK30 at 1000x. (Red circle for void, yellow arrow for fiber ) - 43 -
Fig. 4-3-8 PLM micrographs of PBAT：(a) 150℃, (b) 80℃ (c) RT at 20x (Scale bar = 100 μm), (d) 150℃, (e) 80℃ (f) RT at 50x. (Scale bar = 50 μm) - 45 -
Fig. 4-3-9 PLM micrographs of PHBV：(a) 190℃, (b) 120℃ (c) RT at 20x (Scale bar = 100 μm), (d) 190℃, (e) 120℃ (f) RT at 50x. (Scale bar = 50 μm) - 46 -
Fig. 4-3-10 PLM micrographs of T7V3：(a) 190℃, (b) 120℃ (c) 80℃ (d) RT at 20x. (Scale bar = 100 μm) - 47 -
Fig. 4-3-11 PLM micrographs of T7V3：(a) 190℃, (b) 120℃ (c) 80℃ (d) RT at 50x. (Scale bar = 50 μm) - 48 -
Fig. 4-3-12 LM micrographs of T7V3 at 20x. (The crystal grows from the boundary) - 48 -
Fig. 4-3-13 LM micrographs of sample melted at 190℃ (20x)：(a) PBAT(150℃), (b) PHBV (c) T7V3. (Scale bar = 50 μm) - 50 -
Fig. 4-3-14 LM micrographs of sample melted at 190℃ (20x)：(a) T7V3C10 (b)T7V3C30 (c) T7V3H10 (d)T7V3H30. (Scale bar = 50 μm) - 51 -
Fig. 4-3-15 LM micrographs of sample melted at 190℃ (50x)：(a) T7V3C10 (b)T7V310. (Scale bar = 10 μm) - 51 -
Fig. 4-3-16 LM micrographs of sample melted at 190℃ (20x): - 52 -
(a) T7V3UK10 (b) T7V3UK30 (c) T7V3AK30 (d) T7V3ASK30. (Scale bar = 50 μm) - 52 -
Fig. 4-4-1 (a) TGA and (b) DTG curves of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 54 -
Fig. 4-4-2 DSC curves of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx at 5℃/min-cooled. - 57 -
Fig. 4-4-3 DSC curves of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx at 40℃/min-cooled. - 57 -
Fig. 4-4-4 DSC heating curves of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx after 5℃/min cooling. - 62 -
Fig. 4-4-5 DSC heating curves of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx after 40℃/min cooling. - 62 -
Fig. 4-5-1 Young’s modulus of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 66 -
Fig. 4-5-2 Tensile strength of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 66 -
Fig. 4-5-3 Elongation at Break of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 67 -
Fig. 4-5-4 Flexural modulus of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 70 -
Fig. 4-5-5 Flexural strength of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 70 -
Fig. 4-5-6 Impact strength of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 73 -
Fig. 4-5-7 Storage modulus of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 77 -
Fig. 4-5-8 Tan δ of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 77 -
Fig. 4-6-1 Complex viscosity of PBAT、PHBV、T7V3、T7V3Cx、 T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 80 -
Fig. 4-6-2 Storage modulus of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 80 -
Fig. 4-6-3 Loss modulus of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 81 -
Fig. 4-7-1 Water absorption curve of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 83 -
Fig. 4-7-2 Water absorption of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx s after 168 hr. - 83 -

表目錄
Table 3-1 Sample codes and formulation. - 21 -
Table 4-1-1 Representative TGA data for different treatment of KF. - 31 -
Table 4-2-1 Representative TGA data for different size of cellulose. - 34 -
Table 4-4-1 TGA data of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 55 -
Table 4-4-2 DSC data of 5℃/min cooling. - 58 -
Table 4-4-3 DSC data of 40℃/min cooling. - 59 -
Table 4-4-4 DSC data of 20℃/min heating after 5℃/min cooling. - 63 -
Table 4-4-5 DSC data of 20℃/min heating after 40℃/min cooling. - 64 -
Table 4-5-1 Tensile properties of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 68 -
Table 4-5-2 Flexural properties of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 71 -
Table 4-5-3 Impact property of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 74 -
Table 4-5-4 DMA properties of PBAT、PHBV、T7V3、T7V3Cx、T7V3Hx、T7V3UKx、T7V3AKx、T7V3ASKx. - 78 -

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