由物理汽相傳輸法製備 8-羥基喹啉與 8-羥基喹啉鋁晶體 及其物性探討

Fabrication and Characterization of 8-Hydroxyquinoline and Tris-(8-Hydroxyquinolinate)aluminium Crystals from Physical Vapor Transport

高凡軒(Fan-Hsuan Kao)

指導教授 ： 邱寬城

中原大學/理學院/物理研究所/碩士(2011年)

https://doi.org/10.6840/cycu201100949

摘要

本實驗主要由物理汽相傳輸法 (Physical Vapor Transport, PVT) 製備8-羥基喹啉 (8-Hydroxyquinoline, 8Hq) 與8-羥基喹啉鋁 (Tri (8-hydroxyquinolinato) aluminum, Alq3) 晶體，並利用光激螢光光譜 (PL)、紫外-可見光吸收光譜 (UV-visible)、傅立葉轉換紅外線吸收光譜 (FT-IR)、X光粉晶繞射儀 (XRD) 等分析其特性。首先，我們由PL,FT-IR,及XRD確認購買得到的Alq3粉末為meridional結構，且其晶相為混合相；而經過395℃熱處理後的Alq3粉末為facial 結構 (fac-Alq3)，且其結晶相為δ-phase。接著分別將mer-Alq3及fac-Alq3這兩種粉末以PVT法來觀察本質過飽和區 (Constitutional supersaturation, CSS) 所造成之管壁沉積現象。由改變其間之傳輸氣體 (N2, O2, Dry air or Wet air) 及壓力 (1 ~ 700 torr)，並分別觀察不同粉末源 (mer-Alq3 or fac-Alq3) 所對應的CSS沉積。在管壁溫度約100 ~ 270℃處的CSS沉積物為Alq3，而室溫處CSS沉積物則為8Hq。另外，由mer-Alq3粉末源得到之管壁沉積物之晶相為β-Alq3，而由fac-Alq3粉末源得到的則為α-Alq3。此現象可用活化壁障的圖像來解釋。再者，由固定氣體壓力在400 torr，隨不同傳輸氣體的變化來探討8Hq形成的原因與水氣有強烈的關係。在水氣少的狀況，8Hq的沉積以長條針狀為主；在水氣多的狀況，8Hq則緻密地覆蓋於管壁上，並有較短之針狀結構。

關鍵字

8-羥基喹啉 ； 8-羥基喹啉鋁 ； 傳輸氣體 ； 活化壁障 ； 針狀結構

並列摘要

This paper focuses on the fabrication of tri(8-hydroxyquinolinate)aluminium (Alq3) and 8-hydroxyquinoline (8Hq) crystals from physical vapor transport (PVT) method and the properties of these crystals characterized by photoluminescence (PL), UV-visible absorption spectroscopy (UV-visible), Fourier Transform Infrared Spectroscopy (FT-IR), and Powder X-ray Diffraction (XRD). First, from FTIR, PL, uv-vis, and XRD, the as-received Alq3 powder is confirmed to have meridional structure (mer-Alq3) with mixed phase, and after thermal treatment at 395℃, the facial structure (fac-Alq3) with δ-phase is obtained. Then, by using these two different source (mer-Alq3 and fac-Alq3) powders, the side-wall deposition due to constitutional supersaturation (CSS) in PVT is observed. From a control of different transport vapors (N2, O2, dry air, or wet air) inside the PVT tube with various vapor pressures (1 ~ 700 torr), the side-wall deposition of Alq3 and 8Hq are observed to occur at 100 ~ 270℃ and at room temperature, respectively. Furthermore, the deposition of Alq3 has two different crystal phases depending on the source powder. The β-Alq3 is obtained from mer-Alq3 source powder and α-Alq3 from fac-Alq3 source powder. This phenomenon can be explained by a picture associated with activated barrier crossing diagram. Finally, by using various transport gases but with a fixed pressure of 400 torr, the formation mechanism of 8Hq crystals is found to be strongly related to the content of H2O. In dry gases, needle-like 8Hq crystals are formed preferential; while in wet gases, the side-wall is compactly covered by 8Hq with short needles. The content of H2O inside the PVT tube is believed to play an important role to the dissociation of Alq3 and to the side-wall deposition of 8Hq.

並列關鍵字

PVT ； facial ； Alq3 ； 8Hq ； single crystal ； meridional

參考文獻

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