磷酸鈣生醫陶瓷之連續式合成製程及其於骨填補材之備製研究

Development of Continuous Process for Calcium Phosphate Preparation and Their Preparation in Bone Blocks with 3D Interconnected Pore Structures

梁嘉容(Chia-Jung Liang)

指導教授 ： 楊正昌

共同指導教授 ： 李勝揚

臺北醫學大學/口腔醫學院/生醫材料暨工程研究所/碩士(2011年)

摘要

本研究目的為發展簡化之磷酸鈣鹽類連續式合成法(continuous process)，並將該製程之磷酸鈣產物，結合氫鍵作用力複合體(hydrogen bonding interpolymer complex，IPC)，製備成三維孔洞連通型磷酸鈣骨填補塊材(bone block)。在磷酸鈣鹽類之連續式合成時，僅需控制反應之鈣磷起始原料莫耳比([Ca]/[P] ratio)、pH值與燒結溫度即可備製出各種不同種類之磷酸鈣，再將磷酸鈣與IPC混合後形成感溫性材料，藉由燒結過程之溫度速率控制其膨脹率，並經由燒結將IPC氣化，即可形成不同孔洞大小且具孔洞連通結構之磷酸鈣骨塊。樣品分別應用X光繞射儀、X光螢光分析儀、線性迴歸法、掃描式電子顯微鏡分析其結晶特性、鈣磷莫耳比、BCP之組成含量、孔洞大小。在生物相容性評估上，則以測試細胞之粒線體酶與細胞形態觀察為主。
第四章主要為磷酸鈣鹽類之連續式合成製程，探討連續式合成製程之原料之鈣磷莫耳比、pH值及燒結溫度之調控，對於磷酸鈣鹽類結晶結構之影響，將其繪製成processing window以提供未來加工之依據，並將連續式與傳統批次式合成製程做比較，分析其磷酸鈣產物之物性。第五章主要探討3D孔洞連通骨填補塊材之製程，將連續式合成所製備之BCP與IPC混合後，形成BCP/IPC混合物，藉由調控不同燒結之升溫速率，並在燒結後將IPC氣化，形成3D孔洞連通骨塊，探討升溫速率對於骨塊孔洞大小之影響，及燒結持溫時間對於BCP結晶結構之影響。第六章主要探討不同孔洞大小的塊材，對於細胞生長活性之影響，將四組不同孔洞大小的塊材與小鼠的骨母細胞(MC3T3-E1)共同培養1、7及14天後，測量其細胞活性，並以SEM觀察細胞生長形態。本研究發展連續式合成製程，藉由調控原料之鈣磷莫耳比、pH值及燒結溫度，製備不同種類之磷酸鈣，並將該製程所製備之BCP與IPC混合後，經過升溫速率之調控及燒結後便可獲得不同孔洞大小之骨塊，將塊材與細胞共同培養，觀察孔洞大小對於細胞生長之影響。

關鍵字

連續式合成 ； 磷酸鈣 ； 三維孔洞連通骨填補材

並列摘要

The objective of this study is to develop a continuous process for producing calcium phosphates and prepared 3D pore-connected bone block based on calcium phosphates for bone regeneration. Calcium phosphates were synthesised by continuous process through control [Ca]/[P] ratio of raw materials, pH value and sintering temperature. Then, prepare 3D pore-connected bone block with calcium phosphate and interpolymer complex (IPC). The crystal structure, Ca/P ratio of products, hydroxyapatite (HAp)/??-tricalcium phosphate (??-TCP) ratios of biphasic calcium phosphate (BCP) and pore size were investigated by XRD, XRF, and SEM, respectively. In the chapter 4 of this thesis the development of the continuous process for preparing calcium phosphate bioceramics was introduced. Synthesis of different calcium phosphates by continuous process through controlled [Ca]/[P] ratios of raw materials, pH value and sintering temperature, and synthesis processing window of calcium phosphate reactant was established according the test results. Finally, calcium phosphate products prepared by continuous process were comparing with batch process. Chapter 5 is to investigate the process of 3D pore-connected bone block, mixed BCP with IPC to form a BCP/IPC mixture; the pore size of this mixture was controlled by different heating rates. Gasification of IPC during sintering resulted in the formation of pore-connected biphasic calcium phosphate bone block of different pore sizes. Chapter 6 is to investigate the effect of pore sizes on cell viability. Osteoblasts (MC3T3-E1) were seeded onto bone blocks with different pore sizes, and determination of cell viability after 1, 7 and 14 days culture. In this study, different calcium phosphates can be prepared by continuous process through controlled [Ca]/[P] ratios of raw materials, pH value and sintering temperature. Differect pore sizes of bone block can be obtain by controlled heating rate. Cell viability were influenced by the pore size of bone block.

並列關鍵字

continuous process ； calcium phosphate ； 3D pore-connected bone block

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