CN106308959B - 生物活性玻璃陶瓷纤维和peek树脂复合材料人工牙及制备方法 - Google Patents
生物活性玻璃陶瓷纤维和peek树脂复合材料人工牙及制备方法 Download PDFInfo
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- A61C8/0012—Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy
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Abstract
本发明提供了一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙及制备方法,其制备方法包括四个步骤:制备羟基磷酸钙晶体玻璃陶瓷碎块,制备生物活性玻璃陶瓷纤维,制备生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙,人工牙植入牙槽骨的部分表面层处理。根据本发明方法制备的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙产品,既有足够的力学性能,又具有很好的生物相容性,其力学性能、生物相容性和骨结合强度均大大优于常规人工牙产品,而且整个制备工艺流程简单,操作方便,非常值得大力推广。
Description
技术领域
本发明涉及一种用于人工牙及制备方法,具体是一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙及制备方法,属于牙科医疗器械技术领域。
背景技术
近几年来,国内外口腔种植界对种植和修复美学的努力和研究成了焦点。微创拨牙、不翻瓣或骨膨胀种植,即刻种植,即刻修复,能获得比较理想的临床效果。即刻修复需要初期稳定技术,防止晃动技术,要求种植牙具有加强的穿龈颈部强度,并采用防晃动的倒梯型螺纹,按牙槽窝和唇腭骨板高度和宽度灵活设计个性化一段式种植牙、保证种植牙三维方向的种植导板和对软组织诱导成形的美学基台、美学牙冠等。目前数字技术已经在口腔医学临床应用上得到很大发展,计算机控制机械CAD/CAM和3D打印技术也已经在临床使用,因此临床医学的发展也给材料学提出了更高的要求,一方面要求有生物活性骨组织材料,同时还要求生物活性骨组织材料对负重的疲劳安全性好。
PEEK(聚醚醚酮)树脂是一种生物惰性材料,其表面能较低,很难获得理想的粘接强度,但其具有可靠的生物安全性和优良的机械性能,PEEK树脂复合碳纤维或玻璃纤维材料后,可大大提高强度、刚性和弹性模量,是美国FDA批准可用于临床的医用高分子生物材料。目前,PEEK树脂复合材料已被成功地应用于创伤骨折修复和口腔医学领域。然而碳纤维有着牙科讨厌的黑色,所以碳纤维和PEEK树脂复合材料一般不被牙科采用。
HA(羟基磷灰石)一直是医学工程学科领域研究最多的高分子生物活性材料之一。由于人工HA强度低、脆性大,限制了其在承重方面的应用。用纳米HA和PEEK树脂进行复合,纳米HA会分散在PEEK树脂中,两者之间的结合不是很紧密。因为PEEK树脂是生物惰性材料,而纳米HA被PEEK树脂包裹着,裸露在植入介面的数量不多,导致纳米HA和PEEK树脂复合材料的生物活性较差。如果用纳米HA直接涂覆在PEEK树脂表面,HA涂层无法与PEEK树脂形成较强的结合,而且微小的纳米HA容易被骨组织吸收,其降解的速度和机体骨吸收与机体骨生长很难达到平衡。
高分子生物活性材料除了HA,还有生物活性磷酸钙和生物活性玻璃陶瓷等,其中生物活性玻璃陶瓷为一种多元组合,其利用多元组合结晶相,可以弥补单一晶相的弱点,多晶玻璃大大提高了玻璃母体的强度,复合陶瓷可以有效地促进细胞粘附和增殖。因此生物活性玻璃陶瓷高温熔化后经淬水,退火再熔制形成多晶形产品,更稳定,强度良好。生物活性玻璃陶瓷与骨的结合比HA与骨的结合强度高,是唯一的能够与骨组织成键结合,同时又能与软组织相结合的人工生物材料。
玻璃和陶瓷的最大缺点是脆性大,限制了其应用,但只要通过外力作用把熔融状态下的玻璃拉成丝,形成纤维状,就可变成具有高强度、高模量、耐冲击强度高、抗疲劳性好的材料,高强度玻璃纤维还可用作防弹装甲兵器和舰舶等。而聚醚醚酮和钡玻璃和玻璃陶瓷三元复合纤维材料的弹性模量和热膨胀系数接近人体骨组织。因此,我们选用这些材料进行复合来制备人工牙。
发明内容
本发明的目的是提供一种锶强化生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙及制备方法,用此复合材料制备处理的人工牙,其力学性能、生物相容性和骨结合强度均比常规产品更好。
本发明的具体技术方案如下:
一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙的制备方法,包括以下步骤:
(1)、制备羟基磷酸钙晶体玻璃陶瓷碎块:取化学分析纯级原料SrO 5~15重量份,MgO 0.5~7重量份,CaF2 0.5~1重量份,CaO 33~60重量份,SiO2 22~42重量份,P2O5 11~44重量份,B2O3 0.3~3重量份,将各原料混合均匀,在铂金坩锅中以1400~1500℃熔制后直接淬水得到具有生物活性的羟基磷酸钙晶体主晶相的玻璃陶瓷碎块。
(2)、制备生物活性玻璃陶瓷纤维:将羟基磷酸钙晶体主晶相的玻璃陶瓷碎块进行球磨,制成粒度小于40μm的细粉,再加入5~15重量份的钡玻璃(BGF)细粉,熔混成块或珠后,再放于拉丝坩埚内加热至900~1200℃熔融状态下,用拉丝机拉成所需直径玻璃纤维,玻璃纤维再经退火,得到生物活性玻璃陶瓷纤维。
(3)、制备生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙:取60~80重量份的医用级PEEK树脂粉和20~40重量份长纤维或全长的生物活性玻璃陶瓷纤维,先将生物活性玻璃陶瓷纤维经硅烷处理后在160℃下干燥2小时,再加入PEEK树脂粉,升温到350~400℃熔融后搅拌混合,再经注塑机在400℃的注射温度下注塑或压膜成φ3~φ7mm的棒材,然后根据需要用CAD/CAM设备将棒材加工成不同规格预成品的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙。
(4)、人工牙植入牙槽骨的部分表面层处理:将步骤(3)加工所得的人工牙植入牙槽骨的部分用浓硫酸处理20~60秒,再用丙酮洗涤2分钟,然后再用超声波清洗10分钟,把人工牙植入牙槽骨的部分表面层的PEEK树脂清洗掉10~100μm,使表面层裸露出10~100μm的生物活性玻璃陶瓷纤维头,然后将人工牙消毒备用。
对于制备具有加强穿龈颈部的一段式个性化人工牙种植体,所述步骤(3)也可以采用3D打印的方式进行加工,具体的方法为:取60~80重量份的医用级PEEK树脂粉和20~40重量份短纤维的生物活性玻璃陶瓷纤维,先加热至350~450℃进行混合熔融,再用3D打印机经热熔喷头喷出熔融的复合材料,按个性化需要用计算机控制原有扫描信息设计线路挤出沉积并凝固成型,进而打印出具有加强穿龈颈部、防晃动、具有能诱导软组织成形的美学基台的一段式个性化人工牙种植体。
一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙,其特征是由上述的两种制备方法之一制备而成。
本发明的有益效果为:根据本发明方法制备的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙产品,既有足够的力学性能,又具有很好的生物相容性,其力学性能、生物相容性和骨结合强度均大大优于常规人工牙产品,而且整个制备工艺流程简单,操作方便,非常值得大力推广。
具体实施方式
本发明生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙的制备方法包括以下步骤:
(1)、制备羟基磷酸钙晶体玻璃陶瓷碎块:取化学分析纯级原料SrO 5~15重量份,MgO 0.5~7重量份,CaF2 0.5~1重量份,CaO 33~60重量份,SiO2 22~42重量份,P2O5 11~44重量份,B2O3 0.3~3重量份,将各原料混合均匀,在铂金坩锅中以1400~1500℃熔制后直接淬水得到具有生物活性的羟基磷酸钙晶体主晶相的玻璃陶瓷碎块。
在本步骤中,加入钙(Ca)源可增加生物活性,加入P2O5可益于玻璃陶瓷的形成,加入氟(F)源可以降低熔融温度,加入硅(Si)源加入易于硅烷偶联,加入锶(Sr)源可以增加力学强度,具有网络改性作用。
(2)、制备生物活性玻璃陶瓷纤维:将羟基磷酸钙晶体主晶相的玻璃陶瓷碎块进行球磨,制成粒度小于40μm的细粉,再加入5~15重量份的钡玻璃(BGF)细粉,熔混成块或珠后,再放于拉丝坩埚内加热至900~1200℃熔融状态下,用拉丝机拉成所需直径玻璃纤维,玻璃纤维再经退火,得到生物活性玻璃陶瓷纤维。
在本步骤中,加入钡玻璃可以增加X射线阻射性。
(3)、制备生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙:取60~80重量份的医用级PEEK树脂粉和20~40重量份长纤维或全长的生物活性玻璃陶瓷纤维,先将生物活性玻璃陶瓷纤维经硅烷处理后在160℃下干燥2小时,再加入PEEK树脂粉,升温到350~400℃熔融后搅拌混合,再经注塑机在400℃的注射温度下注塑或压膜成φ3~φ7mm的棒材,然后根据需要用CAD/CAM设备将棒材加工成不同规格预成品的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙。
对于制备一段式人工牙种植体,本步骤也可以采用3D打印的方式进行加工,具体的方法为:取60~80重量份的医用级PEEK树脂粉和20~40重量份短纤维的生物活性玻璃陶瓷纤维,先加热至350~450℃进行混合熔融,再用3D打印机经热熔喷头喷出熔融的复合材料,按个性化需要用计算机控制原有扫描信息设计线路挤出沉积并凝固成型,进而打印出具有加强穿龈颈部、防晃动、具有能诱导软组织成形的美学基台的一段式个性化人工牙种植体。
(4)、人工牙植入牙槽骨的部分表面层处理:将人工牙植入牙槽骨的部分用浓硫酸处理20~60秒,再用丙酮洗涤2分钟,然后再用超声波清洗10分钟,把人工牙植入牙槽骨的部分表面层的PEEK树脂清洗掉10~100μm,使表面层裸露出10~100μm的生物活性玻璃陶瓷纤维头,然后将人工牙消毒备用。
在本步骤中,将人工牙植入牙槽骨的部分表面层的PEEK树脂清洗掉并露出生物活性玻璃陶瓷纤维头,目的是扩大生物活性材料和种牙窝骨质的接触,同时使生物活性材料在降解时强度不会下降,在众多的生物活性玻璃纤维头周围,形成类似于多孔支架,可以支撑骨细胞在支架上迁移,形成对骨组织生长极为有利的环境。
Claims (3)
1.一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙的制备方法,其特征是包括以下步骤:
(1)、制备羟基磷酸钙晶体玻璃陶瓷碎块:取化学分析纯级原料SrO 5~15重量份,MgO0.5~7重量份,CaF2 0.5~1重量份,CaO 33~60重量份,SiO2 22~42重量份,P2O5 11~44重量份,B2O3 0.3~3重量份,将各原料混合均匀,在铂金坩锅中以1400~1500℃熔制后直接淬水得到具有生物活性的羟基磷酸钙晶体主晶相的玻璃陶瓷碎块;
(2)、制备生物活性玻璃陶瓷纤维:将羟基磷酸钙晶体主晶相的玻璃陶瓷碎块进行球磨,制成粒度小于40μm的细粉,再加入5~15重量份的钡玻璃(BGF)细粉,熔混成块或珠后,再放于拉丝坩埚内加热至900~1200℃熔融状态下,用拉丝机拉成所需直径玻璃纤维,玻璃纤维再经退火,得到生物活性玻璃陶瓷纤维;
(3)、制备生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙:取60~80重量份的医用级PEEK树脂粉和20~40重量份长纤维或全长的生物活性玻璃陶瓷纤维,先将生物活性玻璃陶瓷纤维经硅烷处理后在160℃下干燥2小时,再加入PEEK树脂粉,升温到350~400℃熔融后搅拌混合,再经注塑机在400℃的注射温度下注塑或压膜成φ3~φ7mm的棒材,然后根据需要用CAD/CAM设备将棒材加工成不同规格预成品的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙;
(4)、人工牙植入牙槽骨的部分表面层处理:将步骤(3)加工所得的人工牙植入牙槽骨的部分用浓硫酸处理20~60秒,再用丙酮洗涤2分钟,然后再用超声波清洗10分钟,把人工牙植入牙槽骨的部分表面层的PEEK树脂清洗掉10~100μm,使表面层裸露出10~100μm的生物活性玻璃陶瓷纤维头,然后将人工牙消毒备用。
2.根据权利要求1所述的生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙的制备方法,其特征是:对于制备具有加强穿龈颈部的一段式个性化人工牙种植体,所述步骤(3)采用以下方式进行替代:取60~80重量份的医用级PEEK树脂粉和20~40重量份短纤维的生物活性玻璃陶瓷纤维,先加热至350~450℃进行混合熔融,再用3D打印机经热熔喷头喷出熔融的复合材料,按个性化需要用计算机控制原有扫描信息设计线路挤出沉积并凝固成型,进而打印出具有加强穿龈颈部、防晃动、具有能诱导软组织成形的美学基台的一段式个性化人工牙种植体。
3.一种生物活性玻璃陶瓷纤维和PEEK树脂复合材料人工牙,其特征是由权利要求1或2所述的制备方法制备而成。
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