可切削聚合物滲透陶瓷牙科修復材料的制備研究
發(fā)布時間：2018-07-22 11:55
【摘要】：隨著CAD/CAM在牙科修復治療方面的應(yīng)用日益成熟,傳統(tǒng)配套的可切削材料主要為全瓷材料,其脆性大、模量高,對自然牙齒磨耗較大,研制一種性能接近自然牙齒的可切削牙科修復材料具有顯著意義。本研究選用長石陶瓷粉或鋇玻璃粉進行壓制成型、部分燒結(jié)后形成多孔陶瓷,在真空輔助下,利用毛細作用將齒科樹脂雙酚A甲基丙烯酸縮水甘油/二甲基丙烯酸三甘油酯(BisGMA/TEGDMA)真空滲透進多孔陶瓷,樹脂固化后形成樹脂-陶瓷互穿網(wǎng)絡(luò)結(jié)構(gòu),即得到樹脂滲透陶瓷材料,它綜合了樹脂材料和陶瓷材料的優(yōu)勢,具有良好的可切削性,且模量和硬度與自然牙匹配度高。主要工作如下:1.重點開展了基于長石陶瓷粉的多孔陶瓷(3 mm厚)制備和樹脂滲透工藝研究。首先,考察了燒結(jié)條件對長石多孔陶瓷收縮率與孔隙率的影響,并結(jié)合斷面孔隙形貌觀察,確定優(yōu)化的燒結(jié)溫度為755℃,燒制后多孔長石陶瓷的平均孔隙率在20%到25%之間。其次,探究了真空浸漬工藝對樹脂滲透陶瓷材料性能的影響,發(fā)現(xiàn):延長真空保持的時間("g30min)和增加樹脂浸漬的次數(shù)("g3次),有利于樹脂對多孔陶瓷的完全浸潤。第三,用KH570偶聯(lián)劑對多孔陶瓷內(nèi)部孔道進行偶聯(lián)接枝后,有利于樹脂對多孔陶瓷的滲透,有利于樹脂與陶瓷的界面粘結(jié)性,增加樹脂滲透陶瓷材料的力學強度。最后,根據(jù)對所獲得樹脂滲透陶瓷材料的性能(彎曲強度、威布爾模數(shù)、彈性模量、斷裂韌性、維氏硬度、耐磨耗)進行對比研究,確定當BisGMA/TEGDMA比例為6:4時,材料的綜合性能最佳,彎曲強度達到140-150 MPa,威布爾模數(shù)為22.1(2.1),彈性模量為30(4) GPa,斷裂韌性為1.64(0.12) MPam1/2,維氏硬度為5.2(1.3)GPa,磨耗量為8.21(1.33) mm2。由此,得到了一種性能接近自然牙齒的可切削牙科修復材料。2.對比研究了不同厚度(3mm、12mm)長石多孔陶瓷塊的燒結(jié)和樹脂滲透制備。發(fā)現(xiàn)當陶瓷塊的厚度增加后,由于陶瓷塊內(nèi)部散熱速度的限制影響,燒結(jié)溫度需適當降低至725℃,才能保證陶瓷塊良好的多孔結(jié)構(gòu)和適宜的孔隙率。對此12mm的多孔長石陶瓷,選用BisGMA/TEGDMA (6:4)樹脂進行真空輔助滲透,得到的樹脂滲透陶瓷材料,各項性能與前述結(jié)果相近,可采用市面上多數(shù)的CAD/CAM設(shè)備進行切削。3.考慮到長石陶瓷粉的成本較高,本研究還選用齒科復合樹脂常用的鋇玻璃粉進行了探索研究。由于商品化的鋇玻璃粉本身是經(jīng)過硅烷偶聯(lián)劑改性的,經(jīng)過多種制備工藝探索,確定樹脂滲透鋇玻璃陶瓷材料的制備可簡化為壓制得到多孔陶瓷后,直接樹脂滲透,由于樹脂與鋇玻璃粉具有相近的折光指數(shù),樹脂固化后可得到透明的樹脂滲透鋇玻璃陶瓷材料,力學性能發(fā)現(xiàn)還要優(yōu)于長石質(zhì)材料,更接近自然牙齒。4.探索了在長石陶瓷中摻雜結(jié)晶性的氧化鋁或氧化鋯對樹脂滲透陶瓷材料成型工藝參數(shù)和材料性能的影響,發(fā)現(xiàn)它們的加入,對陶瓷燒結(jié)工藝、斷面形貌和孔隙率有明顯影響,但并未能明顯提高材料的力學強度,對提高斷裂韌性有一定作用。本研究制備的兩類樹脂滲透陶瓷材料,性能優(yōu)異,有望作為齒科診療的可切削模型材料和修復材料。
[Abstract]:With the increasingly mature application of CAD/CAM in dental repair and treatment, the traditional complementary Machinable materials are mainly full porcelain materials, which have great brittleness, high modulus and high wear to natural teeth. It is significant to develop a machinable dental restorable material with a performance close to the natural teeth. A porous ceramic was formed after a partial sintering. Under the aid of vacuum, the dental resin, bisphenol A methacrylic acid glycidyl methacrylic acid (BisGMA/TEGDMA) / two glyceryl methacrylate (BisGMA/TEGDMA) was vacuum penetrated into the porous ceramic, and the resin ceramic ceramic interpenetrating network structure was formed after the resin curing, and the resin permeated ceramic material was obtained. It combines the advantages of resin and ceramic materials, has good machinability, and has high modulus and hardness with natural teeth. The main work is as follows: 1. the preparation of porous ceramics (3 mm thick) based on feldspar ceramics and the study of resin permeability are mainly carried out. First, the shrinkage and pore of the porous ceramics of the feldspar ceramics are investigated. The optimum sintering temperature is 755 C, and the average porosity of the porous feldspar ceramics is between 20% and 25% after the burning. Secondly, the effect of vacuum impregnation on the properties of the resin permeable ceramic material is explored, and the time of prolonging the vacuum retention ("g30min") and the increase of the resin impregnation are found. The number ("G3 time") is beneficial to the full infiltration of the porous ceramic with the resin. Third, the coupling grafting of the porous ceramics through the coupling agent of KH570 coupling agent is beneficial to the permeation of the porous ceramics, the interfacial bonding between the resin and the ceramic, and the increase of the mechanical strength of the resin permeated the ceramic material. Finally, the permeability of the resin is obtained. The properties of ceramic materials (bending strength, Weibull modulus, modulus of elasticity, fracture toughness, Vivtorinox hardness, wear resistance) were compared. When the ratio of BisGMA/TEGDMA was 6:4, the composite properties were the best, the bending strength reached 140-150 MPa, the Weibull modulus was 22.1 (2.1), the modulus of elasticity was 30 (4) GPa, and the fracture toughness was 1.64 (0.12) MPam1. /2, the hardness of Vivtorinox is 5.2 (1.3) GPa, and the wear amount is 8.21 (1.33) mm2., thus a machinable dental restorable material with properties close to the natural tooth.2. is obtained. The sintering and resin penetration of different thickness (3mm, 12mm) feldspar ceramic blocks are compared. In order to limit the effect, the sintering temperature should be reduced to 725 C to ensure the good porous structure and suitable porosity of the ceramic block. The porous 12mm ceramics, BisGMA/TEGDMA (6:4) resin is selected for vacuum assisted infiltration, and the resin permeated ceramic materials are obtained. The properties of the ceramics are similar to those of the previous results, and most of the CA in the market can be used. D/CAM equipment is cutting.3. to consider the high cost of feldspar ceramic powder. This study also selected the barium glass powder commonly used in dental composite resin. The commercialized barium glass powder itself is modified by silane coupling agent and through a variety of preparation techniques, the preparation of barium permeable glass ceramic material can be determined. In order to suppress the porous ceramics, the resin permeated directly. As the resin and barium glass powder have a similar refractive index, the resin can get transparent barium permeable glass ceramics after curing, and the mechanical properties are better than the long stone material, which is closer to the natural tooth.4. to explore the crystalline oxidation in the feldspar ceramics. The effect of aluminum or zirconia on the molding process parameters and material properties of the resin permeated ceramic materials has been found. It is found that the addition of them has an obvious influence on the ceramic sintering process, the cross-section morphology and porosity, but it has not obviously improved the mechanical strength of the material and has a certain effect on the improvement of fracture toughness. Two kinds of resin permeable ceramic materials prepared in this study are made. It is expected to be a machinable model material and restorative material for dental diagnosis and treatment.
【學位授予單位】：北京化工大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TQ174.7;R783.1
本文編號：2137387
[Abstract]:With the increasingly mature application of CAD/CAM in dental repair and treatment, the traditional complementary Machinable materials are mainly full porcelain materials, which have great brittleness, high modulus and high wear to natural teeth. It is significant to develop a machinable dental restorable material with a performance close to the natural teeth. A porous ceramic was formed after a partial sintering. Under the aid of vacuum, the dental resin, bisphenol A methacrylic acid glycidyl methacrylic acid (BisGMA/TEGDMA) / two glyceryl methacrylate (BisGMA/TEGDMA) was vacuum penetrated into the porous ceramic, and the resin ceramic ceramic interpenetrating network structure was formed after the resin curing, and the resin permeated ceramic material was obtained. It combines the advantages of resin and ceramic materials, has good machinability, and has high modulus and hardness with natural teeth. The main work is as follows: 1. the preparation of porous ceramics (3 mm thick) based on feldspar ceramics and the study of resin permeability are mainly carried out. First, the shrinkage and pore of the porous ceramics of the feldspar ceramics are investigated. The optimum sintering temperature is 755 C, and the average porosity of the porous feldspar ceramics is between 20% and 25% after the burning. Secondly, the effect of vacuum impregnation on the properties of the resin permeable ceramic material is explored, and the time of prolonging the vacuum retention ("g30min") and the increase of the resin impregnation are found. The number ("G3 time") is beneficial to the full infiltration of the porous ceramic with the resin. Third, the coupling grafting of the porous ceramics through the coupling agent of KH570 coupling agent is beneficial to the permeation of the porous ceramics, the interfacial bonding between the resin and the ceramic, and the increase of the mechanical strength of the resin permeated the ceramic material. Finally, the permeability of the resin is obtained. The properties of ceramic materials (bending strength, Weibull modulus, modulus of elasticity, fracture toughness, Vivtorinox hardness, wear resistance) were compared. When the ratio of BisGMA/TEGDMA was 6:4, the composite properties were the best, the bending strength reached 140-150 MPa, the Weibull modulus was 22.1 (2.1), the modulus of elasticity was 30 (4) GPa, and the fracture toughness was 1.64 (0.12) MPam1. /2, the hardness of Vivtorinox is 5.2 (1.3) GPa, and the wear amount is 8.21 (1.33) mm2., thus a machinable dental restorable material with properties close to the natural tooth.2. is obtained. The sintering and resin penetration of different thickness (3mm, 12mm) feldspar ceramic blocks are compared. In order to limit the effect, the sintering temperature should be reduced to 725 C to ensure the good porous structure and suitable porosity of the ceramic block. The porous 12mm ceramics, BisGMA/TEGDMA (6:4) resin is selected for vacuum assisted infiltration, and the resin permeated ceramic materials are obtained. The properties of the ceramics are similar to those of the previous results, and most of the CA in the market can be used. D/CAM equipment is cutting.3. to consider the high cost of feldspar ceramic powder. This study also selected the barium glass powder commonly used in dental composite resin. The commercialized barium glass powder itself is modified by silane coupling agent and through a variety of preparation techniques, the preparation of barium permeable glass ceramic material can be determined. In order to suppress the porous ceramics, the resin permeated directly. As the resin and barium glass powder have a similar refractive index, the resin can get transparent barium permeable glass ceramics after curing, and the mechanical properties are better than the long stone material, which is closer to the natural tooth.4. to explore the crystalline oxidation in the feldspar ceramics. The effect of aluminum or zirconia on the molding process parameters and material properties of the resin permeated ceramic materials has been found. It is found that the addition of them has an obvious influence on the ceramic sintering process, the cross-section morphology and porosity, but it has not obviously improved the mechanical strength of the material and has a certain effect on the improvement of fracture toughness. Two kinds of resin permeable ceramic materials prepared in this study are made. It is expected to be a machinable model material and restorative material for dental diagnosis and treatment.
【學位授予單位】：北京化工大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TQ174.7;R783.1
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