單水鋁石是製備氧化鋁的常見前驅體礦物。對於具明確疊層型態的單水鋁石原料而言，其層狀結構、礦物學解理面，加上受熱於結構層間發生的脫結晶水及鋁遷移，這為結構層間帶來膨脹壓力及缺陷弱面的產生，再考慮到單水鋁石與γ-Al2O3產物間的結構尺寸及體積差異，等於在原料及剝層動力方面都滿足二維粉末製作條件，然而目前為止卻未有相關作法。本研究認為原因是目前對單水鋁石衍生γ-Al2O3二維片體缺乏了解：1. 由單水鋁石至γ-Al2O3的相轉換內容可能影響外形，以及2. γ-Al2O3不規則外形實際上為原單水鋁石之”碎片化”的結果。因此，儘管兩者間的拓樸關係眾所周知，仍然限制了當前以簡單熱處理製作奈米二維粉末的機會。
　　本研究以具有疊層狀外形之單水鋁石前驅體為粉末原料，成功利用單水鋁石受熱時可能產生的固有剝層現象，配合適當的操作條件，獲得厚度5nm的γ-Al2O3二維粉末。採用不同的升溫速率(0.5、2.5、5.0、10及20oC/min)作為操作變因，等同於在持續升溫的過程中同時考慮溫度與時間兩個變數，觀察到的現象可理解為粉末系統在不同反應時間內，隨溫度升高所發生的動態反應過程。通過有系統的操作法，除了了解晶粒結構轉變內容，也得以了解當系統的熱力學和動力學反應條件改變時，如何影響γ-Al2O3結構於晶粒上的成長方式及特徵，以及反應於所得二維γ-Al2O3的結果。
　　研究結果發現，粉末系統之比表面積值隨溫度上升及釋出結晶水的比例增加，由15 m2/g上升至100 m2/g左右。相變過程中觀察到的晶粒外形與原料單水鋁石維持一致。但於高升溫速率(>5 oC/min)熱處理條件下，當相變完成，所得γ-Al2O3粉末系統存在大量破碎片體，部分表面積應來自因破碎形成的暴露面。因此在厚度評估方面，若以比表面積值100 m2/g換算，由於將所得片體外形假設為完整承襲單水鋁石前驅體，因此所得粉末平均厚度為5-6nm。而當晶粒厚度通過以XRD量測解理方向晶徑來評估，首先單水鋁石(020)由55nm降低至消失前為22nm，表明晶粒隨剝層過程漸次成為薄板狀片體。而升溫速率的影響於生成γ-Al2O3片體厚度顯示出差異，γ-Al2O3 (440)在低升溫速率下小於6nm，在高升溫速率下則大於6nm。經AFM量測低升溫速率下γ-Al2O3二維片體之厚度範圍為5-7.5nm。
　　已知升溫速率影響所得γ-Al2O3片體產生破碎與否，為深究其成因，研究進一步觀察γ-Al2O3核晶結構於晶粒上的成長方式及特徵。結果顯示，隨相變進行，於單水鋁石晶粒上產生鋁陽離子由原來的八面體位點(六配位鋁[VI]Al) 遷移至四面體位點(四配位鋁[IV]Al)，使γ-Al2O3晶胞尺寸沿c軸方向變長，a軸方向縮短。相變先後出現的γ-Al2O3 c/a值不一，核晶間對應的晶格尺寸不一致。在單水鋁石晶粒尚未完全轉換為γ-Al2O3單晶之前，晶粒為一固態膠體複合相系統，由於尚有單水鋁石結構作為緩衝，晶粒保有塑性並得以維持其完整晶形。然而，當相變接近完成時，具有不同晶格尺寸的γ-Al2O3核晶需互相接合，以形成與原單水鋁石晶粒外形相近的 γ-Al2O3單晶(Pseudomorph假形)，否則即會破碎分離，顯然晶粒上核晶間的c/a值差異，即為破碎現象的成因。根據本研究低與高升溫速率兩種熱處理法下所得結果，可以知道相變環境對晶粒外形具有決定性的影響。採<5℃/min升溫速率者，γ-Al2O3核晶在較窄的溫度範圍裡生成，並有較長的時間作晶格尺寸調整，而>5℃/min升溫速率者則否，其結果造成低或高升溫速率下所生成之γ-Al2O3核晶之間，具有相近或差異較大的c/a值，即晶格尺寸。同時，根據a, c軸尺寸變化計算，相對長的反應時間有利於晶面間距縮減，γ-Al2O3於低升溫速率下以較高的結構密度3.644~3.647 g/cm3生成；於高升溫速率下則為3.636~3.640 g/cm3。最終，由於在低升溫速率條件下生成的γ-Al2O3核晶間，經調整至c/a值相近且具有相對高的結構密度，可順利接合得到完整γ-Al2O3晶粒；而在高升溫速率條件下，則出現晶粒破碎現象。
　　至此，我們了解於晶粒上發生的相轉換及γ-Al2O3核晶成長過程，也藉此解析造成晶粒破碎的主要因素為升溫速率。此外，由c/a值變化趨勢可知，γ-Al2O3結構在能量持續輸入下可使各核晶c/a值分布集中並整體向1接近，可達到兩軸相等之立方結構。然而嚴格來說，不論是粉末系統或者單一晶粒上，由於固相反應難以達成均質，各部位無法同時相變，γ-Al2O3的過渡性質又使c/a值分布集中過程難以持續至真正達成c/a=1。因此，若能找到方法使晶粒上之γ-Al2O3結構同步生成，或者適當控制γ-Al2O3穩定度不往δ-Al2O3相變，才有機會由單水鋁石前驅體製備出c/a=1之γ-Al2O3。
　　本研究利用單水鋁石之礦物學特性及相變過程中自然存在的自規性(Self-dimension)尺寸現象，通過熱處理引發剝層現象，以生產奈米級二維粉末。同時，通過有系統的操作法了解其於二維粉末合成中的潛在影響，釐清了先前由單水鋁石生產的γ-Al2O3常出現破碎現象的原因。也指出採用熱輔助剝層技術製備大尺寸或厚度5nm之二維粉末，存在操作條件的限制，這對於優化未來以熱處理作為製備二維奈米粉末之技術至關重要。對於單水鋁石衍生γ-Al2O3中常見的結構議題：四方變形，研究也提出了目前各文獻所得結果的由來，以及實現理想立方結構的具體方向。本文於最後一部分指出，由於晶粒於相變過程中展現出複合相結構，可於相同路徑下製備外形完整的二維單水鋁石-γ-Al2O3複合相晶粒，而γ-Al2O3於原晶粒上的生成細節取決於升溫速率，因此可通過操作法微調所得複合相片狀晶粒之結構密度和組成單元，開闢了一種以複合相結構為晶粒組成特性的創新材料，這種材料將展現出不同相之間的綜合性能，可供未來相關材料的應用或研究方向參考。

In this study, we successfully prepared 5nm thick γ-Al2O3 two-dimensional powder by utilizing the inherent exfoliation phenomenon of boehmite during heating, combined with appropriate operating conditions. Through a systematic approach, we gained valuable insights into the crystal structure transformation, its dependence on the heating rate (phase transformation environment), and the resulting product.
Firstly, we elucidated the potential reasons behind the frequent fragmentation of γ-Al2O3 derived from boehmite and offered practical know-how for heat treatment as a two-dimensional nano-powder preparation technique. Moreover, the crystals displayed a multi-phase structure during the phase transformation process, and a two-dimensional boehmite/γ-Al2O3 crystal with a complete morphology was prepared using the same approach, with the structure finely tuned through various operations such as processing time and heating rate selection. Lastly, concerning the common structural issue in boehmite-derived γ-Al2O3: tetragonal distortion, this research also proposed the origin of the results obtained in the current literature and explored specific directions for achieving the ideal cubic structure.

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