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標題: | 利用大氣電漿熔射蒸汽造孔技術製備氫氧基磷灰石塗層之製程開發與牙科應用 Hydroxyapatite Coatings by Vapour-Induced Pore-Forming Atmospheric Plasma Spraying: Process Development and Dental Applications |
作者: | Yu-Cheng Liu 劉育誠 |
指導教授: | 童國倫(Kuo-Lun Tung) |
關鍵字: | 氫氧基磷灰石,大氣電漿熔射,牙科應用, Hydroxyapatite,Atmospheric Plasma Spraying,Dental Applications, |
出版年 : | 2020 |
學位: | 博士 |
摘要: | 在本篇論文研究中,我們建立並優化了以熱熔射技術來製備氫氧基磷灰石牙科植體的製程,並探討材料對於骨母細胞與骨細胞的相容性。首先,在火焰熔射實驗中,我們發現進料粉體的流動性極其重要,若流動性不好會造成加工不易與加工塗層品質不佳的問題。因此,我們建立了一套造粒技術,使自製粉體都可以達到熱熔射技術的規範。再者,利用仿地質技術,將水置入基材之後,在加工的過程中水蒸汽會破孔而出,造成如火山海島地形的多孔性表面。此結構經由研究發現,更有利於細胞貼附與增生,但由於火焰熔射技術的溫度較低,無法製造出無裂痕的多孔性表面,所以利用能量高的大氣電漿熔射技術來製備多孔性表面。經由電子顯微鏡的檢測後,發現 蒸氣誘導 大氣電漿熔射技術製備的樣品表面無明顯裂痕。為了最適化塗層加工條件,我們調控了不同工作距離、不同工作功率來進行樣品製備。除此之外,我們也利用不同孔徑大小的基材,以更深入了解製備出的蒸汽誘導造孔塗層的不同之處。 從實驗結果發現,不同孔徑大小的基材製備出的多孔性塗層,會隨著基材孔洞變大而變大, 但並不是線性上升。 而且,在體外細胞測試中,也不是越大孔洞的塗層就有最好的細胞增生與分化效果。經此研究得知了,大約 25微米孔洞之基材,會是大氣電漿熔射蒸汽誘導造孔塗層的最佳實驗條件。 不同的氫氧基磷灰石合成條件也是本篇的重點,包含調控溶液酸鹼度與鍛燒溫度。經由 XRD與 FTIR可以發現在調控酸鹼度在 pH = 10時會有最好的氫氧基磷灰石粉體純度,將此粉體利用大氣電漿熔射技術製備塗層來進行測試。此外,對氫氧基磷灰石進行了鍶、鎂與鋅的元素摻雜,並且測試不同濃度下對於細胞的對氫氧基磷灰石進行了鍶、鎂與鋅的元素摻雜,並且測試不同濃度下對於細胞的影響。在經過測試後發現,一定比例的鍶與鎂混摻影響。在經過測試後發現,一定比例的鍶與鎂混摻會有最佳的礦化條件。接著,會有最佳的礦化條件。接著,利用此比例,進行鍶、鎂與鋅的三元素摻雜,利用此比例,進行鍶、鎂與鋅的三元素摻雜,為了解決多孔性醫材不易消毒與感為了解決多孔性醫材不易消毒與感染之問題,鋅的摻雜是非常重要的。染之問題,鋅的摻雜是非常重要的。由結果發現,不論是單獨摻雜鋅元素或是三由結果發現,不論是單獨摻雜鋅元素或是三摻雜含鋅元素的氫氧基磷灰石塗層,都有著不錯的抗菌效果。最後將最適化的合摻雜含鋅元素的氫氧基磷灰石塗層,都有著不錯的抗菌效果。最後將最適化的合成比例利用蒸汽誘導造孔大氣電漿熔射技術,來製備多孔性牙科材料,來了解體成比例利用蒸汽誘導造孔大氣電漿熔射技術,來製備多孔性牙科材料,來了解體外測試的細胞活性與體內測試的礦化與癒合能力。外測試的細胞活性與體內測試的礦化與癒合能力。 In this study, to develop bioactive hydroxyapatite (HAp) coatings for dental and orthopedic applications by thermal spraying techniques, we analyzed the biocompatibility for osteoblasts and pre-osteoblasts. First, we discovered that flowability plays an important role in thermal spraying. If the flowability of the powder is poor, it will lead to a decrease in coating quality as well as coating processing by thermal spraying. Therefore, we established a granulation process with the advantage of improving the flowability of powder to meet the standard of thermal spraying. Furthermore, porous HAp coatings were produced by geomimetic thermal spraying. During melted HAp contacted the titanium (Ti) disc surface, the water behind the porous Ti disc was presently vaporized, and the expansive vapour ran through the flattened melted HAp, which caused the layered, disrupted splats to form a highly porous coating on top of Ti discs. The coating of porous HAp onto Ti disc not only enhanced cell attachment but also improved cell proliferation as well as alkaline phosphatase (ALP) activity. These reactions were beneficial to increase the degree of integration between the implant surfaces and bone tissue. Because the traditional flame spraying was unable to provide sufficient power for the fabrication of porous surface coatings without cracks, atmospheric plasma spraying (APS) with a higher amount of energy was used to deposit porous HAp coatings on Ti discs in this study. The SEM images showed that the vapour-induced pore-forming atmospheric plasma spraying (VIPF-APS) technique did prevent surface cracking, which was a usual feature of conventional APS. Furthermore, we investigated the surface morphology of HAp coating under different operating parameters of APS to optimize the process. We also investigated the characteristic of HAp coatings through the VIPF-APS technique by applying Ti with different mean pore diameters. From our study, we discovered a positive non-linear relation between the mean pore diameter of HAp coating and Ti substrate. These porous coatings further contributed to higher osteoblast proliferation and distinctive alkaline phosphatase activity. As a result of in vitro experiments, porous HAp coating onto Ti substrate with the mean pore diameter to be 10 μm led to the best performance in both proliferation as well as ALP activity of osteoblasts, which also showed that larger pore did not necessarily mean better performance. Optimized conditions to synthesize HAp were also investigated elaborately including adjusting not only pH but also temperature. Higher purity was observed in XRD and FTIR as the condition to be pH = 10 under 800 ℃. Thus, the following samples were all prepared by using this parameter. Moreover, SrMg-HAp coatings were proven that they could not only promote cell and mineralization reactions but also prominently enhanced osseointegration and new bone formation in a beagle dog model on dental implants. HAp, SrMg-HAp, Zn-HAp, and ZnSrMg-HAp coatings were fabricated. Their antibacterial effects, proliferation and differentiation characteristics were further evaluated. The results showed that Zn ions are very important in order to reduce implant-associated and porous implant infections. Also, we investigated the antibacterial effects of Zn-HAp and ZnSrMg-HAp. They both show good performance, which showed Zn ions contribute to antibacterial ability without affecting cell proliferation. Finally, we applied VIPF-APS technique with the optimized operating condition to fabricate porous dental implants to further investigate not only in-vitro cell activity but also in-vivo mineralization and healing ability. |
URI: | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/20265 |
DOI: | 10.6342/NTU202004156 |
全文授權: | 未授權 |
顯示於系所單位: | 化學工程學系 |
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