高分散性奈米粒子合成及複合材料之製備｜國立中央大學博碩士論文系統

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研究生：	陳建偉 Chien-wei Chen
論文名稱：	高分散性奈米粒子合成及複合材料之製備 The synthesis of highly dispersed nanoparticles and preparation of nanocomposites
指導教授：	蔣孝澈 Anthony S.T. Chiang
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程與材料工程學系 Department of Chemical & Materials Engineering
畢業學年度：	98
語文別：	中文
論文頁數：	199
中文關鍵詞：	epoxy 、氧化鋯、水熱法、高折射率複合材料、高分散性奈米粒子、氧化鈦、奈米結晶
外文關鍵詞：	highly dispersed nanoparticles, high refractive index nanocomposite, hydrothermal, epoxy, titania, zirconia, nanocrystal
相關次數：	點閱：13 下載：0
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本研究之最終目標在製備高折射率奈米複合樹脂透明厚膜，其中複合膜中有機材料的部分選用作為LED封裝材料的環氧樹酯ERL-4221(折射率1.5)。無機材料的部份則是選用奈米氧化鈦與奈米氧化鋯，這兩種材料的折射率都在2以上(anatase 相氧化鈦折射率為2.3，氧化鋯則為2.1)，是常見金屬氧化物中折射率較高的，適合被用作提升有機材料的折射率。
初期首要工作為合成高分散性奈米氧化鈦與奈米氧化鋯結晶。為了使奈米複合樹脂厚膜具備透明性及高折射率，因此勢必控制奈米粒子的分散性及結晶大小。我們針對奈米結晶合成過程中的前驅物水解控制、中和pH 及水熱條件(pH、溫度及時間)等作探討，尋找出適合本研究之最終目標的高分散性奈米氧化鈦與奈米氧化鋯結晶之最佳合成條件。
得到高分散性奈米氧化鈦與奈米氧化鋯結晶之後，我們另外研究了TiO2-ZrO2 混合氧化物的合成，試圖瞭解奈米結晶的導入是否具有優勢。最後發現控制鈦源和鋯源的混合方式，經過600℃鍛燒後可以得到ZrTiO4 奈米結晶。
製備奈米複合樹脂必須使奈米結晶與環氧樹酯ERL-4221 均勻混摻或者是彼此產生化學鍵結進而完成交聯硬化，兩者都必須將奈米結晶經過表面改質，方可達成。我們嘗試了油酸、有機胺與矽烷的表面改質，將奈米氧化鈦與氧化鋯結晶分散在有機溶劑中，使其可以與環氧樹酯ERL-4221 均勻混摻。
最後我們選擇將水相分散的奈米氧化鈦與奈米氧化鋯結晶，經過
MPTMS/GPTMS 矽烷改質後，分散在醋酸乙酯中，與環氧樹酯ERL-4221 混摻後，以刮刀塗佈法鍍膜後經過加熱硬化，可以得到奈米TiO2/Epoxy 與ZrO2/Epoxy複合透明厚膜。其中氧化鋯(氧化鈦)含量提高到~45 wt%，折射率可以提升到1.63(1.7)，膜厚2-13 μm (8-35 μm)，而且厚膜之光穿透度在波長600nm 位置時仍有90%以上。

The objective of this research is the preparation of high refractive index transparent nanocomposite thick film. The organic matrix of nanocomposite, epoxy resin ERL-4221 (refractive index is 1.5) is used as an encapsulant of LED. The inorganic material is selected nano-TiO2 and nano-ZrO2 which the refractive index of the two materials are higher than 2 (the refractive index of anatase-TiO2 is 2.3,compared to 2.1 for ZrO2) to enhance the refractive index of organic materials.
The primary work is the synthesis of highly dispersed TiO2 and ZrO2 nanoparticles. For high refractive index transparent nanocomposite, it is necessary to control the dispersity and crystal size of TiO2 and ZrO2. The influences of hydrolysis of precursors, pH value of neutralization and hydrothermal condition(pH, temp. and
time) in the synthesis process of highly dispersed TiO2 and ZrO2 nanoparticles were discussed.
In addition, the preparation of TiO2-ZrO2 mixed oxide was studied. The interesting was whether the advantages of TiO2 and ZrO2 nanocrystals imported for preparation of ZrTiO4 nanocrystal. ZrTiO4 nanocrystal was prepared with the coprecipitation of methacrylic acid-TiCl4 and methacrylic acid-ZrOCl2 by calcination at 600℃.
To disperse nanoparticles and epoxy resin in organic solvent, surface modification of the nanoparticles is pivotal. Surface modification of nanoparticles with oleic acid (sodium oleate), n-hexylamine (dodecylamine) or silane
(3-methacryloyloxy propyl trimethoxysilane and 3-glycidoxy propyl trimethoxysilane) allowed nanoparticles to be dispersed in n-hexane, chloroform and ethylacetate.
The MPTMS&GPTMS-modified TiO2 and ZrO2 dispersions in ethylacetate were blended with epoxy resin ERL-4221 and curing agent. The TiO2/epoxy and ZrO2/epoxy nanocomposite thick film was prepared with MPTMS&GPTMS modified
nanoparticles and epoxy resin ERL-4221 which were dispersed in ethylacetate by blade-coating and thermal curing. The thickness of TiO2/epoxy and ZrO2/epoxy
nanocomposite thick film which contained 15-45 wt% TiO2 or ZrO2 was 2-13 μm and 8-35 μm individually. The refractive index of TiO2/epoxy and ZrO2/epoxy
nanocomposite thick film was up to 1.7 and 1.63 respectively. The optical transmittance of TiO2/epoxy and ZrO2/epoxy nanocomposite thick film was higher than 80% at wavelength of 600 nm.

目錄
摘要............................................................................................................................... I
Abstract ......................................................................................................................... II
致謝..............................................................................................................................IV
目錄..............................................................................................................................VI
圖目錄..........................................................................................................................IX
表目錄........................................................................................................................ XII
1 第一章 高分散性氧化鈦奈米粒子的合成..............................................................1
1-1 前言............................................................................................................1
1-2 氧化鈦性質及應用....................................................................................6
1-3 文獻回顧....................................................................................................9
1-4 實驗方法與結果討論..............................................................................20
1-4-1 四氯化鈦之水解..........................................................................22
1-4-2 中和pH之影響.............................................................................26
1-4-3 水熱條件(pH、溫度與時間)之影響..........................................33
1-4-4 高分散性奈米氧化鈦結晶透明溶膠..........................................37
1-5 結論與建議..............................................................................................45
2 第二章 高分散性氧化鋯奈米粒子的合成............................................................46
2-1 前言..........................................................................................................46
2-2 奈米氧化鋯合成文獻回顧......................................................................51
2-3 實驗方法與結果討論..............................................................................61
2-3-1 氯氧鋯溶液之老化及添加壓克力酸..........................................63
VII
2-3-2 中和pH的選擇及添加保護劑之作用.........................................69
2-3-3 水熱條件對結晶的影響..............................................................75
2-3-4 中性分散之奈米氧化鋯結晶透明水溶膠..................................81
2-4 結論與建議..............................................................................................89
3 第三章 TiO2-ZrO2 複合氧化物之製備..................................................................90
3-1 前言..........................................................................................................90
3-2 文獻回顧..................................................................................................92
3-3 實驗方法與結果討論..............................................................................98
3-3-1 在四氯化鈦和氯氧鋯中加入壓克力酸......................................99
3-3-2 混合奈米氧化鈦和氫氧化鋯....................................................102
3-3-3 混合奈米氧化鈦和奈米氧化鋯結晶........................................105
3-3-4 水熱法製備ZrTiO4 ....................................................................107
3-4 結論........................................................................................................ 111
4 第四章 高折射率奈米TiO2/Epoxy與ZrO2/Epoxy複材之製備...........................112
4-1 前言........................................................................................................112
4-2 文獻回顧................................................................................................114
4-3 奈米粒子的表面改質............................................................................124
4-3-1 利用油酸或油酸鈉進行表面改質............................................128
4-3-2 利用胺類進行表面改質............................................................136
4-3-3 利用矽烷進行表面改質............................................................140
4-4 奈米TiO2/Epoxy與ZrO2/Epoxy複材之製備.........................................143
4-5 結論........................................................................................................149
5 第五章 總結..........................................................................................................156
附錄一 實驗藥品......................................................................................................157
VIII
附錄二 儀器分析......................................................................................................159
參考文獻....................................................................................................................164
IX
圖目錄
圖 1-1 奈米氧化鈦水溶膠合成實驗流程圖............................................................21
圖 1-2 羧酸配位基與金屬鹽的配位模式(M可為Ti或Zr等過渡金屬)86 ................25
圖 1-3 壓克力酸與TiCl4 的配位模式示意圖...........................................................25
圖 1-4 不同pH值中和所得水合物經過水洗以及乙醇清洗後之TGA與DSC圖。A
為TGA熱重損失曲線，B為TGA熱重損失微分曲線圖，C為DSC曲線圖。........30
圖 1-5 不同pH值中和所得鈦水合物經過水洗以及乙醇清洗後之XRD圖。A和B為
pH1.5 中和，C和D為pH4 中和；A和C為經過四次水洗，B和D則是四次水洗後再
經過一次乙醇清洗。..................................................................................................31
圖1-6 pH1.5 和10 中和後所得水合物(TiCl4 添加2mmol MA/g氧化鈦)經過110℃
水熱9 小時(水熱pH1.5 或10)之XRD圖。..............................................................36
圖1-7 奈米氧化鈦結晶粒子酸性水溶膠加入不同有機酸作表面改質後之zeta
potential圖。................................................................................................................40
圖1-8 酸性和中性氧化鈦水溶膠乾燥後粉體之XRD圖。.....................................42
圖 1-9 氧化鈦酸性或中性水溶膠之TEM圖。左圖為氧化鈦酸性水溶膠，右圖為
氧化鈦中性水溶膠。..................................................................................................44
圖 2-1 合成奈米氧化鋯中性半透明水溶膠之標準程序流程圖............................62
圖 2-2 樣品R1-R9 之TGA及DSC圖。A、C和E為TGA圖，B、D和F則為DSC圖。
.....................................................................................................................................67
圖2-3 氯氧鋯水溶液(或有加入MA)經過110℃加熱24 小時之UV-Visible吸收光譜
圖。..............................................................................................................................68
圖 2-4 不同pH下中和所得產物R7-R9 之FTIR光譜。...........................................74
圖 2-5 不同pH下以95℃水熱10 小時後之(A)XRD和(B)DSC圖。.....................78
圖 2-6 不同pH下以110℃水熱不同時間所得產物之XRD圖................................79
X
圖 2-7 pH11.5 溶膠在不同溫度下水熱15 小時後產物之XRD圖..........................80
圖 2-8 奈米氧化鋯結晶粒子酸性水溶膠加入不同有機酸作表面改質後之zeta
potential圖。................................................................................................................84
圖 2-9 奈米氧化鋯中性半透明水溶膠在水熱前與水熱後之XRD及DSC圖。....85
圖 2-10 在pH11.5 下110℃水熱15 小時後以及350℃鍛燒後氧化鋯之Raman光譜
.....................................................................................................................................86
圖 2-11 氧化鋯中性半透明水溶膠之UV-Vis光譜..................................................87
圖 2-12 氧化鋯奈米粒子之TEM照片，從左至右為(a)未經過表面改質；(b)TA表
面改質的氧化鋯中性溶膠；(c)經過CA表面改質的氧化鋯中性溶膠。................88
圖 3-1 不同配製方式的鈦源、鋯源經過酸鹼中和並清洗過濾之沈澱物，在不同
溫度鍛燒後之XRD圖。程序A的鈦源、鋯源配製方式是將TiCl4+MA水溶液以及
ZrOCl2+MA水溶液兩者混合後形成透明水溶液，程序B則是將程序A中所得的水
溶液經過60℃加熱12 小時，程序C則是在不加水的情況下，先將TiCl4-MA溶液
加入ZrOCl2-MA固體中，然後再加入冰水，最後形成一透明水溶液。............101
圖 3-2 酸性或中性氧化鈦奈米結晶溶膠與鋯水合物混合後以及經過鍛燒後之
XRD圖。...................................................................................................................104
圖 3-3 奈米氧化鈦與氧化鋯結晶中性水溶膠混合後經過真空乾燥所得之粉末，
經過鍛燒後之XRD圖，其中(i)as-prepared(ii)500℃(iii)600℃(iv)700℃(v)800℃鍛
燒。............................................................................................................................106
圖 3-4 以第1 種鋯鈦源混合方式得到的鋯鈦前驅物經過110℃水熱15 小時之
XRD圖。由左至右分別為程序A至C中得到的鋯鈦前驅物各自在pH8、10 和11.5
下經過110℃水熱15 小時後之XRD曲線。..........................................................109
圖 3-5 以第1 種鋯鈦源混合方式得到的鋯鈦前驅物經過不同水熱條件後之XRD
圖。由左至右分別為I. 程序A的鋯鈦前驅物在pH8、10 和11.5 下經過180℃水熱
16 小時II. 程序C的鋯鈦前驅物在pH8、10 和11.5 下經過180℃水熱15 小時III. 程
序C的鋯鈦前驅物在pH13 下分別經過110、180 和230℃水熱24 小時後之XRD曲
XI
線。............................................................................................................................110
圖 4-1 文獻中常見的數種烷氧矽烷結構式圖......................................................127
圖 4-2 烷氧矽烷接枝在金屬氧化物奈米粒子表面之反應示意圖。..................127
圖 4-3 以油酸或油酸鈉對奈米氧化鋯進行表面改質之實驗流程圖..................132
圖 4-4 氧化鋯經油酸或油酸鈉表面改質之FTIR圖..............................................133
圖 4-5 氧化鋯經油酸或油酸鈉表面改質之TGA圖...............................................134
圖 4-6 以胺類對奈米氧化鈦進行表面改質及......................................................138
圖 4-7 正十二胺表面改質氧化鈦之TGA圖..........................................................139
圖 4-8 以矽烷對奈米氧化鈦進行表面改質及......................................................142
圖4-9 奈米複合透明膜的TGA圖。其中(A)為TiO2/Epoxy系統；(B)為ZrO2/Epoxy
系統。........................................................................................................................151
圖 4-10 氧化鈦經矽烷改質後以及TiO2/Epoxy複材之FTIR圖............................152
圖 4-11 氧化鋯經矽烷改質後以及ZrO2/Epoxy複材之FTIR圖............................153
圖 4-12 TiO2/Epoxy複合透明膜之光學顯微鏡(400x倍率)照片。由左至右分別為
T-20、T40 和T60 複合透明膜。.............................................................................154
圖4-13 ZrO2/Epoxy複合透明膜之SEM照片。(A) Z-20 和(B) Z-80 複材橫截面以及
(C) Z-20 及(D) Z-60 複材俯視面。.........................................................................154
圖 4-14 TiO2/Epoxy與ZrO2/Epoxy奈米複合透明膜的折射率、透明度和氧化物固
含量關係圖。............................................................................................................155
XII
表目錄
表 1-1 製作奈米粉體的方法.......................................................................................2
表 1-2 二氧化鈦基本性質2,8 .......................................................................................8
表 1-3 以溶凝膠法製備氧化鈦之文獻列表............................................................13
表 1-4 以水熱法製備氧化鈦之文獻列表.................................................................17
表 1-5 奈米氧化鈦穩定懸浮(分散)溶膠之相關文獻列表......................................19
表 1-6 中和產物經過不同溫度鍛燒後之結晶大小................................................32
表 1-7 不同參數製備之氧化鈦酸性溶膠的粒徑分析............................................35
表 1-8 奈米氧化鈦結晶粒子酸性溶膠以不同有機酸改質後之等電點................40
表 1-9 水熱前加入CA對於氧化鈦結晶之影響.......................................................41
表 1-10 不同條件合成的奈米氧化鈦酸性(中性)水溶膠之結晶大小及表面積....43
表 2-1 奈米氧化鋯穩定懸浮(分散)溶膠之相關文獻列表......................................60
表 3-1 合成ZT結晶之相關文獻列表.......................................................................97
表 3-2 不同鋯、鈦源配置方式所得粉體700℃鍛燒後之表面積及孔洞大小...101
表 3-3 不同製備ZT方式所得粉體經不同溫度鍛燒後的晶型..............................106
表 4-1 高折射率複合材料之相關文獻..................................................................122
表 4-2 氧化鋯-正己烷分散液之DLS粒徑測量結果以及氧化鋯粒子表面螯合的
ligand量......................................................................................................................135
表 4-3 常見溶劑之溶解因子..................................................................................135
表 4-4 胺類改質氧化鈦分散於chloroform中之DLS測量結果.............................139
表 4-5 TiO2/Epoxy與ZrO2/Epoxy奈米複合透明膜之組成.....................................150

                                

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