臺灣博碩士論文加值系統

本論文旨在研究利用熔融混煉法製備聚乳酸/滑石粉(改質前後)之複合材料，探討此微米複合材料之加工製程、物理性質、機械性質、熱性質及動態機械性質。實驗使用三-甲氧矽丙基丙烯酸甲酯(APTMS)接枝於滑石粉表面進行改質。用聚乳酸樹酯添加改質滑石粉和未改質滑石粉製備不同的成分克數(每百克的聚乳酸外加上滑石粉之不同克數)之微米複合材料。
探討不同成分克數的Talc和APTMS-m-Talc對聚乳酸樹酯複合材料的形態學(粒徑分析、FT-IR、SEM、ESCA、XRD、Raman)、物理性質(密度、空孔率)、熱性質(TGA、HDT、VST、MI、DSC)、機械性質(硬度、耐磨耗指數、抗張測試、抗折測試及耐衝擊強度)及動態機械性質(DMA)之性能及影響的差異程度。
實驗結果得知，經由FT-IR、TGA、XPS、RAMAN以及XRD測試，可以證實名矽烷偶合劑接枝的成功，並在粒徑分析測試下，證明改質後之Talc粒徑較改質前之Talc粒徑大小要更大，證明矽烷偶合劑改質成功。
在聚乳酸添加Talc與APTMS-m-Talc部分，物理性質的測試，密度皆上升，而空孔率在改質的5phr為最好；在熱性質方面，DSC結晶度隨著Talc及APTMS-m-Talc的添加量增加而上升，VST與HDT、MI熔融指數皆隨著Talc及APTMS-m-Talc的添加量增加而上升；在機械性質測試結果，硬度、耐磨耗指數、抗張模數及抗折模數皆為上升，耐衝擊強度在改質後5phr為最高，抗折強度在未改質5phr為最好，抗折模數在未改質15phr為最好，抗張模數在改質後15phr為最好。
以上結果顯示出聚乳酸樹酯添加未改質Talc粉末有助於提升聚乳酸之抗折模數(15phr最好)、延伸率(15phr最好)。而添加改質過後的APTMS-m-Talc粉末，有助於提升聚乳酸之硬度(15phr最好)、耐磨耗(15phr最好) 、抗張強度(15phr最好)、抗張模數(15phr最好)、結晶度(15phr最好)、熔融指數(15phr最好)。
關鍵詞：聚乳酸、滑石粉、微米複合材料、矽烷偶合劑、改質

This project object is to manufacture polylactic acid (PLA) / Talc (include non-modify and modify) mironcomposites by melt intercalation process, and study the formed by the processing process, physical properties, mechanical properties, thermal properties and dynamic mechanical properties of nanocomposites. The research used 3-Aminopropyl trimethoxysilane (APTMS) grafted silica surface modification. For polypropylene resin add prepared Talc and APTMS -m-Talc mironcomposites with a different number of grams of composition (per 100 grams of polylactide add Talc composition of different number of grams).
Explore the different components of the number of grams of Talc and APTMS-m-Talc mironmeter morphology of polylactic acid resin composites (Particle, FT-IR, SEM, ESCA, XRD、Raman), the optical properties (transmittance), physical properties (Density, Porosity), mechanical properties (Hardness, Wearing, Tensile, Flexure and Impact strength), thermal properties (TGA, HDT, VST, MI, DSC) and dynamic mechanical properties (DMA) for the performance and impact the degree of difference.
Experimental observed results that the success of the grafting of APTMS can be prove by FT-IR、TGA、XPS、RAMAN and XRD tests, it can prove the success of silane coupling agent grafted via; Also that under the particle size analysis, the particle size of the modified Talc is larger than unmodified. It prove that APTMS has been modified successfully..
In the polylactic acid resin added Talc and APTMS-m-Talc part, the physical properties of test, the density increased. While the porosity is better in 5phr of modification; In thermal properites, the crystallinity of DSC is all increased synchronized with the amount of Talc and APTMS-m-Talc. The value of VST, HDR, and MI has increased synchronized with the amount of Talc and APTMS-m-Talc. In the mechanical properties test results, hardness, wear index are all increased, impact strength at the highest 5phr of modification. The tensile modulus was the lowest at 5phr of unmodified Talc, and the elongation was highest at 5phr of unmodified Talc . The flexure of modules was the lowest at 15phr of modified Talc.
The above results show that the addition of unmodified Talc powder to polylactic acid resin helps to increase the density ( 15phr is the best), the void content ( 15phr is the best), and the melt index( 15phr is the best), of polylactic acid. The addition of modified Talc powder helps to increase the density of polylactic acid resin ( 15phr is the best), viod content ( 15phr is the best), crystallinity( 15phr is the best), wearing ( 15phr is the best), melt index( 15phr is the best).
Keywords: Polylactic acid, Talc, Mironcomposites, APTMS, modifacation

摘要……………………………………………….………………...…...……III
Abstract……………………………………………………………………….. V
目錄………………………………………………………………………..…VII
表目錄……………………………………………………………………..…XII
圖目錄………………………………………………………………………XIV
第一章、 緒論…………………………………………………...……. ……..1
1-1 前言…………………………………………………………………….1
1-2 研究動機……………………………………………………………….2
1-3 研究方向……………………………………………………………….4
第二章、文獻回顧……………………………………………………..……6
2-1 聚乳酸Polylactic acid (PLA) …………………………………………6
　　2-1-1 聚乳酸的發展歷史………………………………………………6
　　2-1-2 聚乳酸的結構與製備……………………………………………6
　　2-1-3 聚乳酸的晶體結構………………………………………………8
　　2-1-4 聚乳酸的性質與用途……………………………………………9
2-2　滑石粉…………………………………………………………………10
　　2-2-1滑石粉的簡介……………………………………………………10
　　2-2-2滑石粉的應用……………………………………………………11
2-3　高分子複合材料………………………………………………………13
　　2-3-1高分子複合材料製備方法………………………………………13
　　2-3-2混煉機制與原理…………………………………………………14
2-4　表面改質原理…………………………………………………………16
2-5　歷史回顧………………………………………………………………17
第三章、實驗部分…………………………………………………………26
3-1 實驗材料………………………………………………………………26
3-2 實驗設備與儀器………………………………………………………28
3-3 實驗流程圖……………………………………………………………34
3-4 實驗步驟………………………………………………………………35
　　3-4-1 改質滑石粉APTMS-m-Talc之製備(32) ………………………35
　　3-4-2 聚乳酸樹脂/滑石粉複合材料之製備…………………………36
3-5 材料測試方法…………………………………………………………37
　　3-5-1 傅立葉紅外線光譜分析 (FT-IR) …………………………. 37
　　3-5-2 粒徑分析 ( Particle ) …………………………………………39
　　3-5-3 掃描式電子顯微鏡 ( SEM ) 成像分析………………………41
　　3-5-4 X光繞射分析 ( XRD ) ………………………………………42
　　3-5-5 拉曼光譜分析儀(RAMAN) …………………………………45
　　3-5-6 密度 ( Density ) ………………………………………………47
　　3-5-7 空孔率計算 ( Void Content ) …………………………………48
　　3-5-8 熱重量分析 ( TGA ) …………………………………………49
　　3-5-9 微差掃描式熱分析 (DSC) ……………………………………51
　　3-5-10 熱變形溫度 ( HDT ) …………………………………………54
　　3-5-11 維卡軟化溫度 ( VST ) ………………………………………56
　　3-5-12 熔融指數測定儀（MI）………………………………………58
　　3-5-13 熱機械分析儀 ( TMA ) 熱膨脹係數(CTE)分析……………60
　　3-5-14 硬度 (Hardness) …………………………………………… 62
　　3-5-15 耐磨耗測試 ( Wearing ) ……………………………………64
　　3-5-16 抗張測試 ( Tensile ) …………………………………………66
　　3-5-17 抗折測試 ( Flexure ) …………………………………………68
　　3-5-18 耐衝擊強度測試 ( Impact ) …………………………………70
　　3-5-19 動態機械性質 ( DMA ) 剛性分析…………………………72
第四章、結果與討論………………………………………………………74
4-1 複合材料結構與表面形態學之探討…………………………………74
　　4-1-1 傅立葉轉換紅外線光譜分析 ( FT-IR ) ………………………74
　　4-1-2 粒徑分析 ( Particle ) …………………………………………77
　　4-1-3 掃描式電子顯微鏡 ( SEM ) 成像分析………………………79
　　4-1-4 X光繞射分析 ( XRD) ………………………………………90
　　4-1-5 拉曼光譜分析儀(RAMAN) …………………………………94
4-2 複合材料物理性質之探討……………………………………………98
　　4-2-1 密度之探討 ( Density ) ………………………………………98
　　4-2-2 空孔率之探討 ( Void Content ) ………………………………100
4-3 複合材料熱性質之探討………………………………………………102
　　4-3-1 熱重量分析 ( TGA ) …………………………………………102
　　4-3-2 微差掃描式熱分析 (DSC) …………………………………108
　　4-3-3 熱變形溫度 ( HDT ) …………………………………………113
　　4-3-4 維卡軟化溫度 ( VST ) ………………………………………115
　　4-3-5 熔融指數測定儀（MI）………………………………………117
　　4-3-6 熱膨脹係數之探討（CTE）…………………………………119
4-4 複合材料機械性質之探討…………………………………………122
　　4-4-1 硬度測試 ( Hardness ) ………………………………………122
　　4-4-2 耐磨耗測試 ( Wearing ) ……………………………………124
　　4-4-3 抗張試驗 ( Tensile ) …………………………………………127
　　4-4-3 抗折試驗 ( Flexure ) …………………………………………130
　　4-4-4 耐衝擊強度試驗 ( Impact ) …………………………………133
4-5 複合材料動態熱機械性質之探討……………………………………136
　　4-5-1 動態熱機械分析 ( DMA ) ……………………………………136
第五章、結論………………………………………………………………147
第六章、參考文獻…………………………………………………………152

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