本研究探討由θ-Al2O3相轉換而得之奈米α-Al2O3晶粒的成長熱力學。利用θ-到α-Al2O3相轉換得到α-Al2O3為獲得α-粒體最常用的方法之一。文獻指出θ-到α-Al2O3相轉換係藉孕核成長機制進行。但在成核之後，對α-核晶成長則有不同的看法：以往稱α-核晶的成長是藉相界面推移來進行，然最近研究指出晶粒成長係藉彼此間的聚合來進行。不過，不管是哪一種看法，其論點皆止於初步觀察階段，對於奈米α-晶粒的成長機制、成長過程中顯微構造的發育、晶粒的熱力學特性、及更基礎的晶粒 (包括孕核與成長) 生成熱力學數據的報導則缺。本研究即肇因於此，主要針對 1)初生態α-晶粒的成長行為 (第四章) 及2) 成長過程可能出現之準穩定態α-晶粒的熱力學特性進行觀察 (第五章)。最後再藉1)、2) 之現象配合計算分析建立奈米α-晶粒的成長熱力學模型 (第六章)。
實驗藉熱處理觀察由兩種不同晶徑之θ-Al2O3相轉換而得之α-晶粒的成長行為及過程中的顯微構造變化。在奈米α-晶粒的熱力學特性方面則藉熱處理及機械力處理觀察複合粉末內奈米α-晶粒的相穩定性。再利用現有之熱力學數據，配合實驗結果建立一奈米α-晶粒的成長熱力學模型。
在α-晶粒的成長行為方面 (第四章)：研究結果顯示初生態α-晶粒的成長過程/機制受前相 (母相) 晶粒，即θ-Al2O3，尺寸之影響。當θ-晶粒大於相轉換臨界晶徑 (dcθ, ~ 25 nm) 時，α-核晶在母相 (θ-Al2O3) 內生成後，會以相界面推移的方式成長，新生α-粒體的大小可能受母相尺寸控制。當θ-晶粒小於dcθ時，α-Al2O3則會改以聚合的方式成長，其過程呈三階段跳躍式變化：粒子從核晶之17-20 nm (dcα) 成長至45-50 nm (dp)，接著再繼續成長至最小穩定晶徑 (ds2)，~ 75-100 nm。一旦α-晶粒成長超過ds2，指狀成長可能旋即發生。
在奈米α-晶粒的熱力學特性方面 (第五章)：晶徑< 100 nm之單離α-晶粒在熱力學上屬準穩定態。這類α-晶粒在施以適當熱處理及機械力處理後會有相退變回θ-相的現象。其退回之最低溫度約800oC。當處理溫度大於800oC時，相退變反應所需時間僅數十秒。由於θ-與α-Al2O3密度不同，在相退變發生時，由體積膨脹造成的應力，會使θ-晶粒出現雙晶結構，雙晶面為 (001)。此種具雙晶結構的θ-晶粒再經熱處理又可相變成具雙晶或是鑲嵌構造的α-Al2O3。
在α-晶粒之成長熱力學模型建立方面 (第六章)：研究以實驗結果 (數據) 搭配熱力學計算成功提出一描述α-晶粒成長的熱力學模型，並藉此模型計算得知利用相界面推移與聚合機制成長之α-Al2O3的最小穩定晶徑分別為 ~ 30 (ds1) 與 ~ 75 nm (ds2)。此外，本研究亦藉計算獲得尚未報導之θ-Al2O3晶粒的表面自由能為2.16 J/m2。成長過程中α-晶粒的熱力學狀態會影響晶粒的成長行為：小於或等於最小穩定晶徑 (ds) 的粒子 (∆Gr ≥ 0) 會傾向以單離的方式存在。當成長超過ds後 (∆Gr < 0)，α-晶粒可能會以兩個或兩個以上的單元連接而形成指狀結構。此種指狀晶粒出現的現象與奈米晶粒之初期燒結現象相似。
研究最後以一θ-Al2O3-boehmite為原料，藉其可發生均質反應的特性，成功說明α-Al2O3的晶粒成長過程符合上述之成長模式。本文也相信此舉對奈米α-Al2O3粉末之生產及往後粉末之應用必有關鍵性的幫助。

Growth thermodynamics of nano-scaled α-Al2O3 crystallites transformed from θ-Al2O3 was investigated in this study. θ- to α-Al2O3 phase transformation is one of the most popular used methods for preparation of α-Al2O3 crystallites. It is considered that θ- to α-Al2O3 phase transformation can be achieved by a nucleation and growth process. Once the nucleation of α-Al2O3 occurs, the α-crystallite growth is proposed to be progressed by either interface boundary migration or coalescence processes. However, the understanding of both growth processes for α-crystallites was in the initial stage and the perspective was still ambiguous. There have been no researches focused on the growth mechanisms, the microstructure evolution as well as the thermodynamic characteristics of nano-scaled α-Al2O3 crystallites so far. Furthermore, reports related to the basic thermodynamic data for the formation of α-crystallites was also absent. Therefore, the following objectives were examined in this study: (1) growth behaviors of α-nucleus (Chapter 4), (2) thermodynamic characteristics of nano-scaled α-Al2O3 crystallites formed during the coalescence processes (Chapter 5), and (3) growth thermodynamic models of nano-scaled α-Al2O3 crystallites based on experimental results and theoretical calculations (Chapter 6).
In chapter 4, thermal treatments were employed to investigate the growth behavior as well as the microstructure evolutions of α-nucleus. In chapter 5, powders containing a substantial amount of nano-sized α-crystallites were used as starting materials. Thermal and mechanical treatments were employed to investigate the thermodynamic characteristics of α-Al2O3 crystallites. Moreover, the thermodynamic data referred by the previous studies as well as the experimental results obtained in this study were employed to develop the growth thermodynamic models of nano-scaled α-Al2O3 crystallites in chapter 6.
In chapter 4, it was found that the growth process of α-nuclei was affected by the crystallite size of θ-Al2O3 particles. As the θ-Al2O3 size was larger than the critical size (dcθ, ~ 25 nm) needed for the formation of α-Al2O3 nucleus, the growth of α-crystallites could be performed by interface boundary migration once the α-nucleus formed in the parent phase (θ-Al2O3 crystallites). The size of new-formed α-Al2O3 may be controlled by that of θ-crystallites. As the θ-Al2O3 size was smaller than dcθ, α-crystallite growth could be progressed by coalescence mechanism instead of boundary migration. The coalescent crystallite growth was characterized with quantized size growth. The α-Al2O3 nuclei with sizes 17-20 nm (dcα) coalesced to form α-crystallites of sizes 45-50 nm (dp), then by coalescence of which the stable α-crystallites (ds) with minimum sizes 75-100 nm were obtained. Coalescence of the crystallites of sizes 75-100 nm leads to forming the crystallites with vermicular growth.
In chapter 5, the results demonstrated that discrete α-crystallites of sizes < 100 nm may behave metastable thermodynamically. The nano-sized α-crystallites could take phase-retrogression backward to θ-phase using appropriate thermal and mechanical treatments. The lowest temperature triggered the backward phase transformation was 800oC. And if the crystallites were thermally treated at temperature above 800oC, the α-crystallites experienced phase-retrogression within tens of second. Because of the density difference between θ- and α-phase Al2O3, the strain energies provoked by the volume expansion and shrinkage during the phase transition eventually results in forming the twinned and twinned/or mosaic structure for the θ- and α-Al2O3 crystallites, respectively. The twin plane of twinned θ-Al2O3 is (001).
In chapter 6, thermodynamic models of α-Al2O3 growth were proposed and it demonstrated that the calculations results coincided well with the data observed. It was concluded that the minimum sizes of stable α-crystallites obtained through boundary migration and coalescence processes were ~ 30 nm (ds1) and ~ 75 nm (ds2), respectively. The surface free energy of θ-Al2O3 which has been the first time reported can be 2.16 J/m2. During the growth process, the outline of the particles can be closely related to the thermodynamic state of α-crystallites. α-crystallites with size smaller (∆Gr ≥ 0) and larger (∆Gr < 0) than the stable crystallites (ds) may grow to form discrete and vermiculated particles, respectively. The vermiculated particles were caused by the coalescence of two or more α-crystallites of sizes ds. This study indicated that the phenomena of occurrence of vermiculated particles were similar to that of initial sintering of nanocrystallites.
Finally, θ-Al2O3-boehmite agglomerates were used as staring materials and thermal treatments were employed to demonstrate that the growth process of α-crystallites was well-coincided with the growth model mentioned above. It is believed that the understanding of the growth thermodynamics could be very helpful for the fabrication and application of nano-scaled α-Al2O3 powders in the near future.

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陳智成，氧化鋁-氧化鋯陶瓷複合材料之製備與性質研究，國立成功大學礦冶及材料科學研究所，博士論文，1994年6月。
陳秀雯，利用Boehmite分散及包覆θ-Al2O3粉生產30 -50 nm α-Al2O3，國立成功大學資源工程研究所，碩士論文，2004年6月。
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溫惠玲，由Boehmite製得之氧化鋁粉末的θ→α-Al2O3相轉換，國立成功大學資源工程研究所，博士論文，2000年1月。