臺灣博碩士論文加值系統

從1950年代以來人們已逐步展開對羥基磷灰石(hydroxyapatite；HA)的合成研究，羥基磷灰石為人體骨骼中的磷酸鈣鹽類的主要成分，在骨骼中含量約占69Wt.%，在牙釉質中含量約占96Wt.%，已被大量用以取代醫療材料表面之塗層，並能促使骨質增生與誘導的作用，有效修復缺損組織。用於替代人體組織的生醫材料須具有機械耐久性、優異耐腐蝕性與優良的生物相容性等基本條件，能使植入材料能暫時或永久留於人體而不產生排斥。材料表面塗佈HA的方法有很多種類，而本研究利用循環伏安法(CV)得到適當的沉積電位，以電化學沉積法在鎳鈦合金(Ni-Ti Alloy)表面沉積羥基磷灰石之塗層。
本研究使用雷射共軛焦顯微鏡(LSCM)、掃描式電子顯微鏡(SEM)、能量散射光譜儀(EDS)、X光繞射儀(XRD)，X射線光電子光譜(XPS)等儀器，來測量HA塗層厚度、表面形貌、元素結構及結晶成份等分析。用接觸角量測儀檢測探討表面潤濕性。
掃描式電子顯微鏡(SEM)顯示出在不同沉積時間下呈現出不一樣的塗層形貌。X光繞射儀(XRD)表明沉積的生成物結晶體為DCPA、TCP及HA組成。以不同電壓下進行電沉積，發現2.5V表面鍍層最為均整，電壓過大塗層易剝落，經由提升電解液溫至80℃，HA成核速率加快而形成更微觀形貌結構。X射線光電子光譜(XPS)證明本研究成功備製了羥基磷灰石(HA)之塗層結構。

關鍵詞：鎳鈦合金、電化學沉積法、循環伏安法、羥基磷灰石

Since the 1950s, people have gradually carried out research on the synthesis of hydroxyapatite (HA). Hydroxyapatite is the main component of calcium phosphate salts in human bones, accounting for about 69Wt.% in bones and about 96Wt.% in enamel. It has been widely used to replace the coating on the surface of medical materials , and can promote the role of bone hyperplasia and induction, and effectively repair the defect tissue. Biomedical materials used to replace human tissue must have basic conditions such as mechanical durability, excellent corrosion resistance and excellent biocompatibility, so that the implanted materials can temporarily or permanently stay in the human body without rejection. There are many methods for coating HA on the surface of materials. In this study, cyclic voltammetry (CV) was used to obtain a suitable deposition potential, and a coating of hydroxyapatite was deposited on the surface of Ni-Ti Alloy by electrochemical deposition.
In this study, instruments such as Laser Conjugate Focus Microscopy (LSCM), Scanning Electron Microscopy (SEM), Energy Dispersion Spectrometer (EDS), X-ray Diffraction (XRD), and X-ray Photoelectron Spectroscopy (XPS) were used to measure HA. Analysis of coating thickness, surface morphology, element structure and crystal composition. Surface wettability was investigated with a contact angle meter.
Scanning electron microscopy (SEM) showed different coating morphologies at different deposition times. X-ray diffractometer (XRD) showed that the deposited crystals were composed of DCPA, TCP and HA. Electrodeposition was carried out at different voltages, and it was found that the 2.5V surface coating was the most uniform, and the coating was easy to peel off if the voltage was too high. By raising the electrolyte temperature to 80 °C, the nucleation rate of HA was accelerated to form a more microscopic structure. X-ray photoelectron spectroscopy (XPS) proved that the coating structure of hydroxyapatite (HA) was successfully prepared in this study.

Keywords: Nickel-titanium, Electrochemical Deposition, Cyclic Voltammetry,Hydroxyapatite

摘要 I
ABSTRACT II
目錄 V
圖目錄 VII
表目錄 X
第一章 前言 1
1-1 生物醫用材料產業 1
1-2 生物醫用材料市場 1
第二章 理論基礎與文獻回顧 5
2-1 理論基礎 5
2-1-1 生物醫用材料的簡介 5
2-1-2 生物醫用材料種類與應用 6
2-1-3 生物醫用鈦及鎳鈦合金 8
2-1-4 羥基磷灰石(Hydroxyapatite)介紹 11
2-1-5 羥基磷灰石(Hydroxyapatite)製備方法 12
2-1-6 電化學沉積法 12
2-1-7 生物相容性 13
2-2 文獻回顧 14
第三章 實驗設置與流程 27
3-1 材料準備 27
3-1-1 實驗設置 27
3-1-2 實驗流程 28
3-1-3 試片製備 28
3-1-4 循環伏安法參數設定 28
3-1-5 雙電極電化學沉積法 28
3-2 儀器原理 29
3-2-1 電化學分析儀 29
3-2-2 掃描式電子顯微鏡(SEM)和能量散射光譜儀(EDS) 31
3-2-3 X光繞射儀(XRD) 31
3-2-4 X射線光電子光譜(XPS) 32
3-2-5 雷射共軛焦 32
3-2-6 接觸角量測 33
第四章 實驗結果與討論 45
4-1 電化學沉積羥基磷灰石 45
4-2 不同電壓下沉積羥基磷灰石之結構分析 46
4-3 不同溫度下沉積羥基磷灰石之結構分析 47
4-4 不同時間下沉積羥基磷灰石之結構分析 49
4-4-1 不同時間下沉積羥基磷灰石之SEM分析 49
4-4-2 不同時間下沉積羥基磷灰石之EDS元素分析 49
4-4-3 不同時間下沉積羥基磷灰石之XRD分析 50
4-4-4 不同時間下沉積羥基磷灰石之XPS分析 50
4-4-5 不同時間下沉積羥基磷灰石之成長機制 51
4-5 羥基磷灰石之腐蝕試驗 53
4-6 不同溫度下沉積羥基磷灰石之接觸角分析 54
第五章 結論 76
未來展望 77
參考文獻 78

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