謝國煌臺灣大學：高分子科學與工程學研究所陳偉源Chen, Wei-YuanWei-YuanChen2007-11-292018-06-292007-11-292018-06-292004http://ntur.lib.ntu.edu.tw//handle/246246/62887本研究藉由Hansen model，來估算碳黑-分散液間的作用距離(Interaction distance)與碳黑粒徑的關係，透過此關係來選擇適當的碳黑分散液，以供研究使用。另外為了改善碳黑於UV-可硬化樹脂內的分散性，防止碳黑在樹脂內發生凝聚的現象，以不同的高分子改質方法來改質碳黑的表面，讓碳黑擁有部分高分子的特性，使其能在樹脂內分散均勻，形成薄膜型黑色矩陣。 本論文主要分為兩部分。首先，以Hansen model 作為討論碳黑與液體之間相互作用力的依據，找出液體與碳黑的溶解度參數(Solubility parameter)，計算出碳黑與液體的作用距離，另外以光散射儀量測出碳黑於液體中的粒徑大小，分析兩者的關係，作為碳黑於液體內分散情形的參考依據，結果發現兩者間有正相關性，作用距離越小，碳黑分散佳，粒徑較小。 第二部分是利用不同的聚合物改質碳黑表面，改質的方法包括利用單體(MAA)和起始劑(BPO)、共聚高分子(PMMA -co-MAA)與起始劑(BPO)以及活性聚合物(PSt-T)來改質碳黑的表面，另外用碳黑的良分散液(DMF)與劣分散液(PGMEA)組成不同比例的共溶液，藉此控制碳黑於液體中的粒徑大小，再給於適度的改質。將上述改質後的碳黑離心分離出來，以TGA的結果來推算聚合物於碳黑上的接枝效率，分析其改質情形與粒徑的變化，最後再將碳黑與溶劑和壓克力環氧樹脂混合，配製成黑色矩陣(B.M.) 的樹脂，再以旋轉塗佈的方法，將B.M.塗佈於玻璃基材上，預烤、曝光交聯，形成薄膜型硬化的黑色矩陣，再以AFM觀察碳黑於硬化樹脂內的分散情形與顆粒大小，分析其變化情形。研究結果顯示可以透過選取適當的溶液組合，與不同的碳黑改質方法，來控制於樹脂型黑色矩陣內碳黑粒子的大小，與分散穩定度，達到薄型樹脂型黑色矩陣的性質。In the present research the relationship between the interaction distance and the particle size of carbon blacks was established by using the Hansen model. With this relationship suitable liquids can be chosen for dispersion of carbon blacks. In addition, polymer grafting on carbon blacks was performed to obtain more uniform dispersion in UV-curable resins, so that thin film black matrix can be fabricated. First, with the solubility parameters of dispersion liquids and carbon blacks, the interaction forces between them could be estimated with the Hansen model. Besides, the particle size of carbon blacks was measured by using light scattering. The relationship between the particle size of carbon blacks and the interaction distance could then be established. The results indicated that good correlation between them could obtained, and the smaller the interaction distance, the better the dispersion of carbon blacks and the smaller the particle size. The modified carbon blacks were then dispersed in the cosolvent of DMF (good dispersion liquid) and PGMEA (poor dispersion liquid). By adjusting the composition of the cosolvent, the particle size of the modified carbon blacks could be tailored. In addition, modification on the dispersed carbon blacks was performed with grafting of monomer (MAA) and copolymer (PMMA-co-MAA) by the initiator BPO, and grafting of living polymer (PSt-T). The modified carbon blacks were separated from the liquid by centrifuge and the amount of grafting was estimated. The modified carbon blacks were further mixed with epoxyacrylate resins to form black matrix resins, which were then spin-coated on glass substrate to form thin film. After baking and UV-curing, thin film black matrix was obtained. The dispersion of carbon blacks in the matrix was investigated by AFM. The results indicated that ultra-thin black matrix could be successfully fabricated with the method discussed above.目錄 中文摘要…………………………………………………………………I Abstract……………………………………………………….………...III 目錄………………….…………………………………………………V 表索引………………………..………………………………………...IX 圖索引……………………………………………...……...……………XI 第一章：緒論……………………………………………………………1 第二章：文獻回顧………………………………………………………4 2-1 碳黑……………………………………………………………….4 2-1.1 碳黑的分類…………………..………………………4 2-1.2 碳黑的基本特性……………………………………..8 2-1.3 碳黑的光電特性……………………………………11 2-2分散與溶解……………………………………………….12 2-3 粉粒體粒徑量測-雷射繞射法…………………………17 2-3.1量測原理…………………………………………….17 2-4碳黑表面改質與應用………………………………...………….23 2-4.1 高分子接枝碳黑的原理與方法………………..…23 2-4.1.1 高分子接枝上碳黑 .………………………25 2-4.1.2 由碳黑表面進行接枝反應.…………..……25 2-4.1.3高分子與碳黑表面官能基反應 …………..25 2-4.2 碳黑於液體中的分散性………………..………….26 2-4.2.1 碳黑的分散性與溶解度參數關係……..…26 2-4.2.2 表面改質碳黑於溶劑中的分散性………27 2-5 UV-可硬化樹酯………………………………………….27 2-6 感光性高分子應用於黑色矩陣……………………….29 第三章 實 驗…………………………………………………..32 3-1實驗藥品………………………………………………….32 3-2實驗儀器………………………………………………….40 3-3 實驗流程…………………………………………………46 3-3.1 各種液體與碳黑的分散關係……………….…….46 3-3.2 聚合物接枝包覆碳黑………………………..…….47 3-3.3 聚合物接枝包覆碳黑(含有穩定自由基)……..…48 3-3.4 共聚高分子接枝包覆碳黑…………………….....49 3-3.5 樹脂型黑色矩陣之製備…………………………..50 3-4實驗方法………………………………………………….51 3-4.1 液體與碳黑的分散關係………………….………..51 3-4.2 帶有自由基高分子改質碳黑……………………..51 3-4.2.1製備帶有穩定自由基的高分子……….……..51 3-4.2.2改質碳黑………………………………………..52 3-4.3 UV可硬化樹脂之製備……………………….….…53 3-5實驗條件……………………………………………..……54 3-5.1碳黑與不同溶液的分散情形………………….…...54 3-5.2 PS-T之製備……………………………………….…54 3-5.3聚合物接枝包覆改質碳黑……………….…………55 3-5.4改質碳黑與UV-可硬化樹脂混合形成黑色矩陣...57 3-6實驗分析…………………………………………….…….58 3-6.1 熱重損失分析儀 (TGA) ………………….…..….58 3-6.2 穿透式電子顯微鏡 (TEM)…………………..…...59 3-6.3 掃瞄式電子顯微鏡 (SEM)…………………….….59 3-6.4光散射分析儀 (Light Scattering Analyzer)………59 第四章 結果與討論…………………………………….………60 4-1碳黑分散性與液體溶解度參數之關係………………...60 4-2改質碳黑的粒徑變化…………………………………….67 4-2.0改質碳黑條件總覽表……………………………….69 4-2.1以共聚合物和起始劑改質碳黑……………………70 4-2.2以單體和起始劑改質碳黑………………….………74 4-2.3單體改質共溶液內的碳黑………………………….78 4-2.4以活性聚合體改質碳黑………….…………………82 4-3.3 不同的碳黑改質方法與接枝包覆效率的影響….86 第五章 結 論……………………………………………………87 參 考 文 獻……………………..……………………………...911629363 bytesapplication/pdfen-USUV可硬化樹脂碳黑Hansen model黑色矩陣Carbon BlackUV curable resinBlacthesishttp://ntur.lib.ntu.edu.tw/bitstream/246246/62887/1/ntu-93-R91549004-1.pdf