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研究生:鄭文賢
研究生(外文):Wen-Hsieh Cheng
論文名稱:磷酸鈣粉末製程及性質研究
論文名稱(外文):Process and Properties of Calcium Phosphate Powder
指導教授:朱建平朱建平引用關係陳瑾惠
指導教授(外文):Chien-Ping JuJiin-Huey Chern Lin
學位類別:碩士
校院名稱:國立成功大學
系所名稱:材料科學及工程學系碩博士班
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2004
畢業學年度:92
語文別:中文
論文頁數:88
中文關鍵詞:磷酸鈣溼式化學反應煅燒
外文關鍵詞:calcinewet-chemical reactioncalcium phosphate
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  人類能直立行走靠得是骨骼為支架稱起人體,但當因遺傳、疾病、意外及損害造成骨骼損傷、缺陷而喪失其功能性時,則需人工骨骼材料加以填補修復,現今人工骨骼材料相當廣泛,包括金屬、陶瓷跟高分子等材料,而其中以磷酸鈣鹽類具生物可吸收性的特性最受各界所注目,相關研究也日益增加。

  在所有的磷酸鈣鹽類中又以三鈣磷酸鹽及四鈣磷酸鹽最受重視,除了具生物可吸收性外,其初期硬化具高強度、可注射性、最終產物和人體骨相似均為其特點。然而現今製造三鈣磷酸鹽及四鈣磷酸鹽方式大多為固相燒結方式配合研磨獲取磷酸鈣粉末,不僅耗時費力,機械耗損及汙染問題也是需克服的條件。

  本實驗為利用溼化學析出方式,先以各種不同種類之鈣磷化合物來獲取與四鈣磷酸鹽鈣磷比例相似的析出前趨物,再配合煅燒方式燒除揮發性物質得到四鈣磷酸鹽粉末。在析出反應過程中當pH=12所獲得的前趨物鈣磷比例接近2,於高溫煅燒後粉末為分散粉末,粉末形態平均為大小約82nm的球狀體,和現今燒結製造方式具相當大差異。
  The human can walk because the skeleton support human body. It needs article skeleton materials to repair the damage position when the skeleton get hurt and lose its work by hereduty, disease, accident and damage. There are several kinds of article skeleton materials, include of metal, ceramic and polymer materials. All of them are focus on calcium phosphate because it could be absorb by human body.

  The calcium phosphate, tricalcium phosphate and tetracalcium phosphate, not only the property of absorption by human bady but also its high initial compress strength, injectable, and the final production closed to the human skeleton. But the disadvantage of them are that the process to produce tri- and tetra- calcium phosphate were solid-state reaction with high temperature sintering reaction. After sintering , it also needs to grind to tiny particle.

  This research used wet-chemical precipitation reaction method to get precursor that similar to TTCP with different calcium source and phosphate source, following to calcine to get tetracalcium phosphate. From the precipitation reaction process at pH=12, we can get the precursor with Ca/P range close to 2 and after calcining the poeder were all disperse , and the average range of disperse powder were 82nm.
摘要 ………………………………………………………………… I
總目錄 ………………………………………………………………… II
圖目錄 ………………………………………………………………… V
表目錄 ………………………………………………………………… VII

第一章 前言…………………………………………………………… 1
1-1 前言…………………………………………………………… 1
1-2 實驗目的……………………………………………………… 2

第二章 理論基礎與文獻回顧………………………………………… 6
2-1 生醫材料敘論………………………………………………… 6
2-2 奈米材料製作方式…………………………………………… 7
2-2-1 化學析出法…………………………………………………… 8
2-2-2 溶膠-凝膠法………………………………………………… 9
2-2-3 水熱法………………………………………………………… 12
2-3 氫氧基磷灰石特性…………………………………………… 13
2-3-1 氫氧基磷灰石基本特性……………………………………… 13
2-3-2 氫氧基磷灰石結構…………………………………………… 13
2-4 非晶質磷酸鈣鹽類…………………………………………… 14
2-4-1 非晶質磷酸鈣鹽類的基本性質……………………………… 14
2-4-2 非晶質磷酸鈣鹽類的結構…………………………………… 15
2-5 四鈣磷酸鹽…………………………………………………… 15
2-5-1 四鈣磷酸鹽的基本性質……………………………………… 15
2-5-2 四鈣磷灰石的製作方式與熱性質…………………………… 16
2-6 成核結晶理論………………………………………………… 17
2-6-1 成核熱力學理論……………………………………………… 17
2-6-2 晶體成長……………………………………………………… 18

第三章 實驗步驟……………………………………………………… 27
3-1 實驗原料簡介………………………………………………… 27
3-2 新材料開發測試流程………………………………………… 27
3-2-1 TTCP粉末製作流程…………………………………………… 27
3-2-1-1 不同鈣源及磷源測試………………………………………… 27
3-2-1-2 不同鈣源及磷源,及添加其他離子影響測試……………… 28
3-2-1-3 其他析出反應測試…………………………………………… 29
3-2-1-4 煅燒處理測試………………………………………………… 31
3-2-2 磷酸鈣粉末基本性質………………………………………… 32
3-2-2-1 X光繞射分析…………………………………………………… 32
3-2-2-2 掃瞄式電子顯微鏡分析……………………………………… 32
3-2-2-3 霍式紅外線光譜(FTIR)分析………………………………… 32
3-2-2-4 能譜儀(EDS)分析……………………………………………… 33

第四章 實驗結果與分析………………………………………………… 42
4-1 不同鈣源和磷酸根源測試……………………………………… 42
4-1-1 不同鈣源和磷酸根源析出物結果……………………………… 42
4-1-2 不同鈣源和磷酸根源析出粉末XRD相分析…………………… 43
4-1-3 不同鈣源和磷酸根源析出粉末紅外線光譜分析……………… 44
4-1-4 不同鈣源和磷酸根源析出粉末EDS分析……………………… 46
4-1-5 不同鈣源和磷酸根源析出粉末SEM分析……………………… 47
4-2 不同鈣源及磷源及添加其他離子影響測試結果……………… 60
4-3 其他析出反應測試結果………………………………………… 65
4-3-1 有機溶液析出反應測試結果…………………………………… 65
4-3-2 OCP粉末碳酸根化測試結果…………………………………… 65
4-4 煅燒處理測試結果……………………………………………… 70
4-4-1 不同鈣磷比例煅燒處理結果…………………………………… 70
4-4-2 不同升溫速率煅燒處理結果…………………………………… 71
4-4-3 低溫煅燒處理結果……………………………………………… 72

第五章 結論……………………………………………………………… 82

第六章 參考資料………………………………………………………… 84
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張立得、牟季美, 奈米材料和奈米結構,滄海書局,中華民國91年6月
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