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研究生:陳美蒨
研究生(外文):Mei-Chien Chen
論文名稱:牙科居家漂白對複合樹脂填補材料的影響
論文名稱(外文):Effects of home-bleaching on composite resin restorative materials
指導教授:李士元李士元引用關係
指導教授(外文):Shyh-yuan Lee
學位類別:碩士
校院名稱:國立陽明大學
系所名稱:臨床牙醫學研究所
學門:醫藥衛生學門
學類:牙醫學類
論文種類:學術論文
論文出版年:2007
畢業學年度:95
語文別:中文
論文頁數:134
中文關鍵詞:居家漂白複合樹脂水分子擴散退化拉曼光譜
外文關鍵詞:home-bleachingcomposite resinwater diffusiondegradationRaman spectrum
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牙齒漂白是美容牙科中一項普及的項目,過去的研究發現居家漂白會造成複合樹脂材料的退化,然而其作用機制卻仍不清楚。
本實驗採用臨床常用的三類複合樹脂,包括了兩種混成型複合樹脂(3M Z100, Filtek Z250)、一種微粒型(Filtek Z350)以及一種聚丙烯酸改良式樹脂(compomer, Dyract AP),將其製作成15 x 1 mm大小的圓盤狀試片(n = 30)後部分進行水分子擴散檢測,以測量各材料的吸水度及水溶解度。其他試片在聚合七天後隨機分成兩組,一組進行居家漂白的實驗組,每天浸泡在10%過氧尿素八個小時持續28天,另一組則浸泡去離子水當控制組。在居家漂白處理前及處理後第七天、十四天、二十一天、二十八天分別檢測試片表面性質,包括微硬度、粗糙度及顏色的表現,並由各組隨機取樣進行掃瞄式電子顯微鏡觀察複合樹脂的表面特性,以及透過拉曼光譜分析其化學結構的改變。
結果發現本實驗採用的複合樹脂其水分子擴散程度不同,吸水度最大的是Z350,其次是Z100和DAP,最小的是Z250。各材料在進行居家漂白後退化程度也不同,以聚丙烯酸改良式複合樹脂DAP退化程度最為顯著,有最大的顏色改變、粗糙度增加,其次是Z100,對於Z250及Z350影響程度甚小。而各材料漂白後的微硬度表現結果不同,DAP與Z100漂白後硬度軟化,但是Z250和Z350卻有相對於控制組稍大的硬度表現。
在電子顯微鏡下可見漂白劑對各種材料皆造成較控制組顯著的表面退化。拉曼光譜分析顯示漂白後的複合樹脂其化學結構有所改變,漂白後的混成型及微粒型複合樹脂其C=C雙鍵(ω = 1638 cm-1)振動減少而C-O單鍵(ω = 1200 ~ 1355 cm-1)振動增加,推測其破壞機制是漂白劑的氧化攻擊。對於聚丙烯酸改良式樹脂而言,漂白後造成羧酸鹽類(carboxylic salts)的產生以致於碳酸根(CO2-)對稱性分子振動的降低(ω = 1335 ~ 1440 cm-1),推測其破壞的機制可能在於漂白劑加速水分子的擴散,以進行次級酸鹼反應產生羧酸鹽類。
在本實驗的限制下,居家漂白對於複合樹脂影響的程度有材料上的差異,可能和複合材料有機基質的吸水度、填料粒子的配置,以及聚合硬化機制有關。至於微硬度的檢測並不是觀察複合樹脂表面退化的一個適合的指標,採用電子顯微鏡觀察或是光譜分析可能更恰當。在臨床上進行居家漂白處理前的病例,應該避免使用聚丙烯酸改良式樹脂填補,至於使用其他複合樹脂材料則應預先考量其顏色變化與結構的破壞,因為漂白劑會有加劇複合樹脂退化的情況,可能促進磨耗增加、牙菌斑堆積及美觀上的疑慮。
Tooth bleaching has become popular in the esthetic dentistry. Previous literatures found that home-bleaching might increase degradation of composite resins. However the mechanism is still unclear.
Four composite resins were enrolled in the study, including two light-polymerized hybrid composites (3M Z100 and Filtek Z250), one microfilled composite (Filtek Z350), and one polyacid-modified composite (compomer, Dyract AP). Thirty standardized disc specimens (15 x 1 mm) of each material were made and stored in distilled water for 7 days, in which 5 specimens of each material was used to measure the water sorption and solubility. Twenty specimens were randomly divided into two groups, in which one group was immersed in 10% carbamide peroxide solution for 8 hours per day for 28 days, and the other group was stored in distilled water as control. Surface properties, including Knoop microhardness, roughness and CIELab values of each specimen was measured, before bleaching treatment and repeatedly at intervals of 7, 14, 21 and 28 days, respectively. The rest specimens were used for examination under SEM and Raman spectroscope in order to investigate the surface characteristics and polymeric structures.
The results showed that Z350 had higher water sorption then Z100 and DAP, while Z250 had the least. The impacts of home-bleaching on composite resin degradation were also different. DAP had the greatest degradation with the most color changes and roughness increase compared with the control group, followed by Z100, while Z350 and Z250 had the least degradation subjected to bleaching treatment. Bleaching impacts on microhardness of composite resins were material dependant. Bleached DAP and Z100 were softer than the control group, whereas bleached Z350 and Z250 were harder.
With the observation of the surface of specimens under SEM, all materials tested had more degradation profile after home-bleaching compared to the control group. The Raman spectrum revealed that home-bleaching treatment changed the chemical polymeric structures of the composite resins. The aliphatic C=C bond vibration (ω = 1638 cm-1) was reduced and carbonyl bond vibration (C-O, ω = 1200 ~ 1355 cm-1) was increased in hybrid and microfilled composite resins. This denoted that oxidation reaction could be a possible mechanism of degradation of composite resins subjected to home-bleaching treatment. Meanwhile the CO2- asymmetric stretching vibration (ω = 1335 ~ 1440 cm-1) was reduced and carboxylic salts was increased in Raman spectrum of polyacid-modified composite resin. The possible reason is that home-bleaching accelerated the water diffusion and thus enhanced the acid-base neutralization of polyacid-modified composite resin.
Within the limitation of this study, the degradation effects of home-bleaching on composite resins were material dependant, which might be related to the water diffusion of resin matrix, filler type and setting mechanism of these materials. SEM observation and Raman spectrum analyses seem to be good tools to evaluate the degradation of bleached composites, while microhardness of composite resins was not a good indicator. Applying the findings of this study, polyacid-modified composite resins should be avoided to restore the teeth before home-bleaching therapy, and also the discoloration and polymeric change of other composites should be anticipated, since home-bleaching could accelerate the degradation of composite resins and consequently increase the surface roughness, poor esthetics and tendency of wear.
目錄……………………………………………………………………1
圖表目錄………………………………………………………………4
中文摘要………………………………………………………………8
英文摘要………………………………………………………………10
一、緒論………………………………………………………………12
二、文獻回顧…………………………………………………………13
(一)、漂白的作用及其機制…………………………………………13
(二)、漂白對於複合樹脂的影響……………………………………16
1.複合樹脂的組………………………………………………………16
2.複合樹脂的退化及其表面性質和化學結構………………………21
3.漂白對於複合樹脂的影響及其機制………………………………25
三、研究動機與目的…………………………………………………29
四、實驗材料與方法…………………………………………………30
(一)、實驗設計………………………………………………………30
(二)、實驗材料………………………………………………………31
1.複合樹脂材料及試片樣本製作……………………………………31
2.居家漂白劑的配置…………………………………………………31
3.複合樹脂試片的承載模托製作……………………………………32
4.實驗分組……………………………………………………………32
(三)、複合樹脂進行水分子擴散檢測………………………………33
1.複合樹脂水分子擴散的測量………………………………………33
2.複合樹脂水分子擴散的計算………………………………………33
3.統計分析……………………………………………………………33
(四)、複合樹脂進行居家漂白處理…………………………………34
(五)、複合樹脂表面性質檢測與化學結構光譜分析………………34
1.複合樹脂表面粗糙度測試…………………………………………34
2.複合樹脂表面微硬度測試…………………………………………35
3.複合樹脂表面顏色測試……………………………………………35
4.複合樹脂表面電子顯微鏡觀察……………………………………37
5.複合樹脂化學結構光譜分析………………………………………38
6.統計分析……………………………………………………………39
五、結果………………………………………………………………40
(一)、複合樹脂水分子擴散檢測……………………………………40
(二)、複合樹脂表面粗糙度測試……………………………………40
(三)、複合樹脂表面微硬度測試……………………………………41
(四)、複合樹脂表面顏色測試………………………………………41
(五)、複合樹脂表面電子顯微鏡觀察………………………………44
(六)、複合樹脂化學結構拉曼光譜分析……………………………45
(七)、結果總結………………………………………………………48
六、討論………………………………………………………………50
(一)、實驗設計的考量………………………………………………50
(二)、從拉曼光譜分析探討居家漂白對於複合樹脂化學結構的影響
…………………………………………………………………………57
(三)、居家漂白對於複合樹脂顏色的影響…………………………63
(四)、居家漂白對於複合樹脂微硬度的影響………………………65
(五)、電子顯微鏡下觀察居家漂白對於複合樹脂的影響…………68
(六)、居家漂白對於複合樹脂影響的可能機制……………………69
(七)、本實驗與過去相關文獻研究的比較…………………………71
(八)、本實驗臨床上及材料學上的應用……………………………74
(九)、本實驗的限制與未來展望……………………………………75
七、結論………………………………………………………………77
八、參考文獻…………………………………………………………126




圖表目錄
圖一:牙科居家漂白…………………………………………………78
圖二:臨床常用複合樹脂其常見樹脂基質的單體化學結構式……79
圖三:矽烷耦合劑……………………………………………………80
圖四:複合樹脂的自由基聚合作用…………………………………81
圖五:聚合物的退化…………………………………………………84
圖六:複合樹脂圓盤狀試片樣本……………………………………85
圖七:居家漂白劑的配置……………………………………………85
圖八:複合樹脂試片承載模托的製作………………………………86
圖九:水分子擴散檢測………………………………………………86
圖十:表面粗糙度測量………………………………………………87
圖十一:微硬度測量…………………………………………………87
圖十二:顏色測量……………………………………………………88
圖十三:掃瞄式電子顯微鏡(JEOL JSM-5300)……………………89
圖十四:拉曼光譜分析………………………………………………89
圖十五:拉曼光譜實驗組與控制組內部標準化……………………90
圖十六:量化分析複合樹脂拉曼光譜的波段………………………91
圖十七:四種複合樹脂的吸水度及水溶解度………………………92
圖十八:四種複合樹脂的粗糙度測量結果…………………………93
圖十九:四種複合樹脂的微硬度測量結果…………………………94
圖二十:四種複合樹脂的顏色測量結果……………………………95
圖二十一:以CIE L*a*b*三個參數分析各樹脂顏色改變(ΔE)……96
圖二十二:複合樹脂明度的改變……………………………………97
圖二十三:複合樹脂紅綠顏色的改變………………………………98
圖二十四:複合樹脂黃藍顏色的改變………………………………99
圖二十五:聚丙烯酸改良式樹脂DAP掃描式電子顯微鏡下的觀察100
圖二十六:混成型複合樹脂Z100掃描式電子顯微鏡下的觀察……101
圖二十七:混成型複合樹脂Z250掃描式電子顯微鏡下的觀察……102
圖二十八:微粒型複合樹脂Z350掃描式電子顯微鏡下的觀察……103
圖二十九:複合樹脂T0天的拉曼光譜波形…………………………104
圖三十: 複合樹脂T14天的拉曼光譜波形…………………………104
圖三十一:聚丙烯酸改良式樹脂的羧酸功能基單體………………106
圖三十二:微粒型複合樹脂的填料粒子配製………………………107
圖三十三:複合樹脂進行自由基聚合反應後的聚合結構…………108
圖三十四:過氧化氫分解自由基的氧化作用………………………108
圖三十五:氫鍵對於羰基化學共振的影響…………………………109
圖三十六:聚合物的彈黏性變形 (viscoelastic deformation) 109
圖三十七:異分子聚合物的內部增塑………………………………110

表一:化學共軛鏈系統………………………………………………111
表二:根據不同填料粒子分類的複合樹脂…………………………111
表三:本實驗的材料表………………………………………………112
表四:本實驗的儀器表………………………………………………113
表五:四種複合樹脂的吸水度及水溶度……………………………113
表六:吸水度及水溶解度的單因子變異數分析結果及Tukey比較.114
表七:粗糙度的三維變異數分析結果(3- way ANOVA of roughenss)
……………………………………………………………….115
表八:複合樹脂T0、T7、T14、T21、T28五個時間點的粗糙度測量
……………………………………………………………….115
表九:微硬度的三維變異數分析結果(3- way ANOVA of hardenss)
……………………………………………………………….116
表十:複合樹脂T0、T7、T14、T21、T28五個時間點的微硬度測量
……………………………………………………………….116表十一:複合樹脂實驗組與控制組微硬度的比較…………………117
表十二:顏色的三維變異數分析結果
(3- way ANOVA of ΔE, ΔL*, a*, Δb*)………………….118
表十三:複合樹脂T0、T7、T14、T21、T28五個時間點顏色…….120
表十四:複合樹脂實驗組與控制組顏色改變的比較………………121
表十五:複合樹脂T0、T7、T14、T21、T28五個時間點實驗組
與控組 的顏色變化量比較……………………………….122
表十六:複合樹脂T0、T7、T14、T21、T28五個時間點明度的改變
(△L*)……………………………………………………….122
表十七:複合樹脂T0、T7、T14、T21、T28五個時間點紅(+a*)綠
(-a*)顏色的改變……………………………………………123
表十八:複合樹脂T0、T7、T14、T21、T28五個時間點黃(+b*)藍
(-b*)顏色的改變……………………………………………124
表十九:T14天拉曼光譜標準化後的各波段量化分析…………….125
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