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研究生：	謝家豐 Hsieh, Chia-Feng
論文名稱：	奈米纖維素強化聚乳酸複合材料的應用研究 Applications of nanocrystalline cellulose reinforced polylactic acid (PLA) composites
指導教授：	施士塵 Shi, Shih-Chen
學位類別：	碩士 Master
系所名稱：	工學院 - 機械工程學系 Department of Mechanical Engineering
論文出版年：	2019
畢業學年度：	107
語文別：	中文
論文頁數：	110
中文關鍵詞：	聚乳酸、奈米纖維素、雙螺桿混煉、射出成型、磨耗性質、單面膠黏拉伸試驗
外文關鍵詞：	Polylactic acid, nanocrystalline cellulose, Injection molding, wear properties, single lap shear test
相關次數：	點閱：218 下載：3
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天然纖維增強聚合物複合材料的應用範圍在各個工程領域迅速發展。本研究主要探討奈米纖維素(nanocrystalline cellulose, CNC)的添加對聚乳酸(polylactic acid, PLA)複合材料的機械性質、熱穩定性、磨耗特性和親疏水特性以及應用於工程塑膠的可行性。
研究顯示CNC在沒有經過改質的狀態下直接與PLA複合的強化效果並不理想，即便設計螺桿組態來改善分散，最終結果也相當有限。而結晶度因為過度聚集抑制了異質成核的發生；拉伸結果在含量1 wt.%CNC時得到最優越的韌性斷裂，隨著含量增加，其中的楊氏係數與斷裂強度分別上升6.2%和2.1%。而CNC有助於增加抗磨耗性，PLA/CNC在磨耗時受CNC的保護，因此磨耗行為有所提升。膠黏部分透過電漿改質，使表面同時產生化學與物理作用，進而提升20.9%的最大膠黏抗剪切強度。

關鍵字：聚乳酸、奈米纖維素、雙螺桿混煉、射出成型、磨耗性質、

Nanocrystalline cellulose (CNC) is a good candidate of reinforcement for composites, The application of nanocrystalline cellulose as fabric or structural reinforcements widely introduced in the a variety of industries. This studies the properties of CNC by using twin screw extrusion to combine PLA and 1, 3, and 5wt.% CNC and produces ASTM test specimens through inject molding. The composite material obtained through inject molding sees an increase in the strength compared to pure PLA. However, from the experiments, it was discovered that CNC aggregates within PLA and as a result has a limited enhancement to the strength of PLA. In addition, an improvement in the wear resistance of PLA/CNC composite material was observed. It was also observed that adding 5wt.% CNC to the composite material can reduce its friction coefficient. In addition, the adhesive shear strength of the composite was also improved by atmospheric plasma treatment when nozzles were used at a distance of 12mm. Surface roughness was reduced by 62%, thereby increasing the shear strength of the composite.

key words : polylactic acid, nanocrystalline cellulose, injection molding, wear test, single lap shear test

總目錄
口試合格證明	i
摘要	ii
誌謝	ix
總目錄	x
表目錄	xiv
圖目錄	xvi
第1章 緒論	1
1.1 前言	1
1.2 研究動機	5
第2章 文獻回顧	8
2.1 高分子特性	8
2.1.1 生物降解高分子簡介	8
2.1.2 聚乳酸簡介Polylactic acid	9
2.1.3 奈米纖維素 (Cellulose nanocrystalline )	10
2.1.3.1 奈米纖維素製備簡介	11
2.1.4 高分子的機械性質	12
2.2 高分子加工簡介	13
2.2.1 高分子流變特性	13
2.2.2 黏度與溫度關係	16
2.2.3 雙螺桿混煉(Twin screw extrusion)	17
2.2.3.1 螺桿組態(Screw configuration)	18
2.2.3.2 同向咬合(co-rotating)與異向咬合(counter rotating):	18
2.2.3.3 同向咬合與異相咬合的混煉效果	19
2.2.3.4 螺桿組態設計	19
2.2.4 射出成型(Injection molding)	20
2.2.4.1 射出成形過程	21
2.3 聚乳酸複合奈米纖維素	23
2.4 膠黏應用及設計	25
2.4.1 黏著定義與黏著劑種類	25
2.4.2 濕潤性與接觸角	26
2.4.2.1 潤濕性(Wettability)	26
2.4.2.2 接觸角與Young’s方程	27
2.4.3 表面粗糙度與影響接觸角的因素	28
2.4.4 影響表面形貌參數	29
2.4.4.1 振幅參數(Amplitude parameters):	29
2.4.4.1.1 中心線平均粗糙度(Roughness average，Ra)	29
2.4.4.1.2 最大波峰高度(Maximum peak height，Rp)	30
2.4.4.1.3 粗糙度幾何平均值(Root-mean-square【RMS】roughness, Rq)	31
2.4.4.2 綜合參數(Hybrid parameters):	31
2.4.4.2.1 振幅分佈之偏斜度(Skewness，Rsk)	31
2.4.4.2.2 振幅分佈之陡峭度(Kurtosis，Rku)	32
2.4.5 低溫電漿處理提升表面自由能	33
2.4.6 單面黏合剪切	36
2.5 單面膠黏抗剪切強度與低溫大氣電漿	37
第3章 實驗規劃	40
3.1 實驗流程	40
3.2 實驗方法	41
3.2.1 實驗材料	41
3.2.2 成型加工設備簡介	46
3.2.3 熱分析	51
3.2.4 機械性質分析	52
3.2.5 迴轉式-磨耗試驗機(Pin-on-disk)	54
3.2.6 低溫大氣電漿	55
3.2.7 表面形貌分析	57
3.2.8 表面親疏水特性與表面自由能分析	60
第4章 實驗結果與討論	61
4.1 熱分析	61
4.1.1 熱重分析(TGA)	61
4.1.2 差示熱掃描分析(DSC)	62
4.2 抗拉強度分析	64
4.2.1 拉伸斷裂點	64
4.2.2 純PLA與PLA/CNC的機械性質	64
4.3 拉伸斷裂面形貌分析	70
4.4 磨耗性質分析	72
4.4.1 不同距離下的耐磨性分析	72
4.5 低溫大氣電漿提升表面親水性分析	77
4.5.1 不同高度的電漿處理影響表面粗糙度	78
4.5.2 固定高度的電漿處理之表面粗糙度	84
4.5.3 不同含量的CNC影響PLA的表面自由能	88
4.6 搭接剪切強度分析	95
4.6.1 電漿改質影響膠黏剪切拉伸強度	95
4.6.2 膠黏斷裂面的失效模式	99
第5章 結論	102
5.1 總結	102
參考文獻	104

表目錄
表 1 1 Property chart for basic polymers for gearing	4
表 2 1 射出成型過程(上)	21
表 2 2 射出成型過程(下)	22
表 2 3 拉伸結果 [26]	23
表 2 4 溶液表面張力表[39]	35
表 3 1 PLA原始機械性質總表	41
表 3 2 CelluForce NCCTM 產品之性質	42
表 3 3 3MTM Scotch-WeldTM Epoxy adhesives	43
表 3 4 電木布基(棉布)-C	44
表 3 5尼龍(MC901-齒輪級)	45
表 3 6射出加工條件	48
表 3 7表面粗糙度值對照表[50]	59
表 4 1 TGA分析結果	62
表 4 2純PLA與PLA/CNC複合材料的DSC數據總結	63
表 4 3純PLA與PLA/CNC的最大抗拉強度(σy)、最大斷裂強度(σB)、楊氏模數(E)與伸長率(%)	66
表 4 4 電漿處理前的表面粗糙度	80
表 4 5不同高度下的電漿處理之表面粗糙度	81
表 4 6 接觸角量測電漿處裡後的表面親水衰退過程	83
表 4 7表面未經過電漿處理的表面粗糙度數據總表	85
表 4 8表面經過電漿處理的表面粗糙度數據總表	85
表 4 9 純-PLA表面未經過電漿改質的接觸角與表面自由能	91
表 4 10 PLA/1 wt.%CNC表面未經過電漿改質的表面自由能	91
表 4 11 PLA/3 wt.%CNC表面未經過電漿改質的表面自由能	92
表 4 12 PLA/5 wt.%CNC表面未經過電漿改質的表面自由能	92
表 4 13 純PLA表面經大氣電漿改質後的接觸角與表面自由能	93
表 4 14 PLA/1 wt.%CNC表面經大氣電漿改質後的表面自由能	93
表 4 15 PLA/3 wt.%CNC表面經大氣電漿改質後的表面自由能	94
表 4 16 PLA/5 wt.%CNC表面經大氣電漿改質後的表面自由能	94
表 4 17 PLA/CNC材料的膠黏抗剪強度與表面自由能比較	98


 
圖目錄
圖 1.1 PLA應用的演進	2
圖 1.2 工程塑膠分類[2]	3
圖 1.3 常見的塑膠齒輪	5
圖 1.4 實驗魚骨圖	7
圖 2.1 聚乳酸合成過程 [6]	9
圖 2.2右旋乳酸(D-lactic acid)與左旋乳酸(L-lactic acid) [7]	10
圖 2.3 (a)單纖維素鏈重複單元的示意圖(b)纖維素纖維結晶和無定形的配置(c)酸水解後的奈米纖維素溶解了無序段[11]	11
圖 2.4 應力-應變關係圖	13
圖 2.5流體元素	14
圖 2.6 流動曲線圖	15
圖 2.7黏度與溫度關係圖	16
圖 2.8單螺桿混煉示意圖	18
圖 2.9 雙螺桿咬合方式	19
圖 2.10本次研究使用的雙螺桿組態	20
圖 2.11 壓出螺桿與射出螺桿比較	21
圖 2.12 雙螺桿組態與混煉擠出機 [26]	24
圖 2.13 不同方法製備薄膜(a)溶液澆鑄法(b)旋轉塗佈法和薄膜的SEM微影圖(50μm ×500)(c)溶液澆鑄法(d)旋轉塗佈法 [27]	25
圖 2.14界面膠黏示意圖	26
圖 2.15 黏著劑種類	26
圖 2.16 固、液、體三項界面示意圖	27
圖 2.17 (a) Wenzel與(b) Cassic-Baxter固液界面示意圖	29
圖 2.18中心線平均粗糙度 [33]	30
圖 2.19 最大波峰高度 [33]	30
圖 2.20粗糙度幾何平均值 [33]	31
圖 2.21 振幅分布之偏斜度 [33]	32
圖 2.22振幅分布陡峭度 [33]	33
圖 2.23 單面搭接膠黏剪切應力分佈 [41]	36
圖 2.24在1英寸寬和1/4英寸厚的鋼帶上進行試驗 [40]	37
圖 2.25 三種典型的膠黏失效模式 [43]	38
圖 2.26 PLA表面經過大氣電漿在不同噴嘴高度與進給速率下的剪切測試之膠黏斷裂面 [44]	39
圖 3.1 實驗流程圖	40
圖 3.2 同向雙螺桿混煉機	46
圖 3.3台中精機 Vs-50k射出成形機 [45]	48
圖 3.4 射出成形模具(a)ASTM標準試片(b)模穴為120*90*2 mm模具	49
圖 3.5射出成型成品	49
圖 3.6 除濕乾燥機	50
圖 3.7 QC-H51A2拉伸試驗機	52
圖 3.8標準試片(a)ASTM D638 Type I [47]與(b)ASTM D5868 [48]	53
圖 3.9 Epsilon延伸計	53
圖 3.10 正齒輪及螺旋齒輪受力點	55
圖 3.11磨耗試驗機	55
圖 3.12 噴射式電漿噴頭設計	56
圖 3.13掃描S型路徑	57
圖 4.1純PLA與PLA/ 1、3、5wt.%CNC的TGA分析曲線	61
圖 4.2  純PLA與PLA/1、3、5wt% CNC的DSC熱分析曲線	63
圖 4.3 拉伸試驗試片斷裂結果	64
圖 4.4 奈米纖維素與噴霧式乾燥法 [14]	66
圖 4.5 Pure PLA之應力-應變	67
圖 4.6 PLA/1 wt% CNC之應力-應變	67
圖 4.7  PLA /3 wt.%CNC之應力-應變	68
圖 4.8  PLA/ 5 wt.%CNC之應力-應變	68
圖 4.9 市售的工程材料與純PLA和PLA/CNC的拉伸強度比較	69
圖 4.10拉伸斷裂面；500μm，100倍(a)純PLA(b)PLA/1 wt.%CNC(d)PLA/3 wt.%CNC(c)PLA/5 wt.%CNC	71
圖 4.11 固定荷重1.5 N和轉速239 rpm下，電木、尼龍和PLA/CNC系列在100、200、300 m的磨耗體積(μm3)與摩擦係數(μ)變化	74
圖 4.12電木、尼龍和PLA/CNC系列的磨耗率	75
圖 4.13固定荷重1.5 N和239 rpm下，材料磨耗所對應之消散能	75
圖 4.14 電木、尼龍和PLA/CNC系列在100、200、300 m下的磨耗痕跡(上)	76
圖 4.15電木、尼龍和PLA/CNC系列在100、200、300 m下的磨耗痕跡(下)	77
圖 4.16電漿處理後的表面形貌(A)(B)(C)處理高度為6 mm(D)(E)(F) 處理高度為12 mm(G)(H)(I) 處理高度為18 mm	80
圖 4.17 電漿處理後的表面形貌(A’)(B’)(C’) 處理高度為6 mm(D’)(E’)(F’) 處理高度為12 mm(G’)(H’)(I’) 處理高度為18 mm	81
圖 4.18 電漿噴頭距離試片6 mm的接觸角變化	82
圖 4.19電漿噴頭距離試片12 mm的接觸角變化	82
圖 4.20電漿噴頭距離試片18 mm的接觸角變化	83
圖 4.21 未過電漿處理的2D表面粗糙度輪廓和表面未經過噴式電漿處理的表面形貌3D輪廓	86
圖 4.22經過電漿處理後的2D表面粗糙度輪廓和表面經過噴射式電漿處理的表面形貌3D輪廓	87
圖 4.23 未經過電漿改質前各含量的接觸角	89
圖 4.24 經過電漿改質後各含量的接觸角	89
圖 4.25 未經過電漿處理的表面自由能	90
圖 4.26 經過電漿處理的表面自由能	90
圖 4.27電漿處理前單面搭接膠黏拉伸的剪切負荷與位移曲線圖	97
圖 4.28電漿處理後單面搭接膠黏拉伸的剪切負荷與位移曲線	97
圖 4.29電漿表面改質前後的搭接剪切應力變化比較	98
圖 4.30 黏著劑厚度0.5 mm的抗剪切斷裂面(a)未經過電漿處理(b)經過電漿處理	100
圖 4.31 透過黏著劑將剪切力從一個構件傳遞到另一個構件[40]	101
圖 4.32 (左)單面搭接剪切和剝離應力的典型變化[73]，(右)等高線圖顯示(a)軸向應力(b)剪切應力和(c)單面搭接接頭的剝離應力[71]	101
                                    

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