CN117064579A - 一种氮化硅陶瓷种植体及制备方法 - Google Patents
一种氮化硅陶瓷种植体及制备方法 Download PDFInfo
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Abstract
本发明提供了一种氮化硅陶瓷种植体及制备方法,具体包含一种种植体结构及其光固化3D打印成型方法,通过改进氮化硅光固化浆料配方及工艺,可实现脱脂阶段的快速升温,有效提高浆料稳定性和生产效率,能够制备复杂结构种植体,种植体底部的十字尖瓣可以在植入初期稳定种植体位置,与骨组织形成有效锚固。
Description
技术领域
本发明属于医疗器械增材制造领域,具体涉及一种氮化硅陶瓷种植体及制备方法。
背景技术
近年来,陶瓷材料在医疗器械领域应用广泛,氮化硅陶瓷与其他牙科陶瓷相比具有更高的强度和断裂韧性,其磨损率远远低于金属和其他陶瓷材料,同时密度比氧化铝、氧化锆和钛合金等更小。此外氮化硅具有良好的抗菌性。但是在陶瓷种植体的成型技术上,传统成型技术如凝胶注模、等静压等难以制备复杂的多孔结构,不利于增加骨种植体与骨组织的结合面积和结合强度。采用3D打印的方法解决陶瓷材料成型问题,是一种快速、高效的方法。3D打印的原理是通过逐层添加材料来形成实体,其特点为无需机械加工,无需模具,可制造传统方式难以形成的复杂、精细结构。其中,光固化3D打印是发展最早、最成熟的3D打印技术,其基本原理是利用光敏树脂的光固化性,将光源经过图形编程,投射到树脂表面,使树脂中含有的自由基成分分解,进而引起光敏树脂的聚合,从而在紫外光对应的位置形成图形结构,其优点包括精度高、打印对象表面光滑、打印速度快等。
三周期极小曲面(TPMS)结构被证实是一种合适的仿生的骨种植体结构,TPMS表面非常光滑,没有点阵多孔结构的尖锐转折或连接点,整体结构互相贯通。在自然界的一些生物组织中,已经发现了与TPMS非常相似的结构,通过在圆柱直径方向和轴向方向进行孔结构的梯度设计,可以更好的提高骨种植体的骨整合性和结合强度,同时配合3D打印技术实现精密的增材制造。
CN 107586136 B公开了一种3D打印氮化硅陶瓷的方法,且利用打印过程中的双层刮刀成型技术,可使β相氮化硅取向排布,经脱脂烧结后,可获得具有复杂形状的织构化氮化硅陶瓷。所制备的氮化硅零件具有优异的可靠性、力学性能、热学性能、耐磨性等,脱脂的方法为在氮气、氩气、真空或者空气条件下,将坯体以0.5~2℃/min的速率升温至600~800℃,保温1~3h。烧结的方法为在氮气气氛,气压为0.1~200MPa的条件下,将脱脂后的坯体以3~10℃/min的速率升温至1600~1900℃保温1~10h。
CN 106674828 A公开了一种3D打印氮化硅陶瓷材料及其制备方法,该制备方法包括:1 )将高岭土、膨润土、氮化硅、硼酸、草木灰、三氧化钼、纳米铝、玻璃纤维和水进行混合,接着进行煅烧以制得煅烧产物;2)将聚偏氟乙烯、甲基纤维素、硅烷偶联剂与煅烧产物进行混合以制得基料;3)将基料进行研磨以制得3D打印氮化硅陶瓷材料。该3D打印氮化硅陶瓷材料的液相表面张力小进而使得陶瓷制品的表面的裂纹少;同时该制备方法原料易得、工序简单。其升温工序为将混合物自15~35℃以0 .5~0 .8℃/min的速率升温至150~200℃并保温20~40min,接着以1.5~2.5℃/min的速率升温至300~380℃并保温30~40min,最后以0.8~1℃/min的速率升温至470~520℃并保温。
CN 112174676 A提供一种氮化硅髋臼杯的制备方法,包括:S1、提供固相含量为35~45vol%的氮化硅陶瓷料浆,料浆包括含量为料浆总质量 0.3~2.8%的分散剂;S2、将光固化3D打印机的打印区域温度设置为30~45℃,打印料浆,得到髋臼杯坯体;S3、对坯体脱脂、烧结,得到氮化硅髋臼杯。
CN 116063083 A提供了一种光固化浆料的快速脱脂方法,热脱脂处理工艺为10~150℃下升温速度0.1~0.5℃/min,保温70~80min;150~300℃下升温速度0.5~1℃/min,保温55~65min;300~450℃下升温速度1~1.5℃/min,保温40~50min;450~1000℃下升温速率5~10℃/min,保温20~30min。
上述3D打印器件设计和浆料工艺,排胶速度普遍极慢,尤其是在300℃以下的低温脱脂阶段。在陶瓷光固化3D打印领域,浆料配方和应用结构的设计是两个关键问题,主要是为了解决陶瓷光固化浆料的打印、排胶、烧结效率以及提高应用性能。传统的氮化硅陶瓷浆料粘度较高,树脂硬度大,交联度低,排胶速度慢且易开裂,不易成型复杂结构。本发明提供了一种可以以3~15℃/min速率全程升温的快速脱脂配方,粘度低效率高,可以成型复杂结构的仿生骨种植体。
发明内容
针对以上问题,本发明提供一种3D打印氮化硅陶瓷种植体,一方面,种植体具有仿生孔结构;另一方面,该种植体采用一种光固化3D打印方法成型,本发明提供的3D打印浆料配方可以较快的升温速率进行脱脂排胶,生产效率高,力学性能良好。
本发明提供一种3D打印氮化硅陶瓷种植体,包括如下步骤:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1~5:1的比例混合,100~200 rpm 低速球磨96~126小时,然后干燥过200目筛网,得到粉体A;S2、将预聚体B和单体C、光引发剂以一定质量比均匀混合得到混合光敏树脂D;S3、将D、惰性稀释剂E、分散剂、流平剂以一定体积比均匀混合后,得到光敏树脂F;S4、将A和F均匀混合后得到陶瓷浆料G;S5、将G利用光固化设备进行3D打印成型得到打印坯体H;S6、将H以3~15℃/min的升温速率在空气环境下进行升温并保温一段时间得到脱脂坯体I;S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到陶瓷种植体J。
具体的,所述球磨过程中的球料比优选4:1的质量比,球磨工艺优选100rpm球磨120小时,过筛后得到流动性佳的混合粉体A。
具体的,所述预聚体B是聚氨酯丙烯酸酯(PUA)、环氧丙烯酸酯(EA)中的一种或几种,单体C为季戊四醇四丙烯酸酯(PPTTA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、1,6-己二醇二丙烯酸酯(HDDA)、二缩三丙二醇二丙烯酸酯(TPGDA)、甲基丙烯酸羟乙酯(HEMA)中的一种或几种,惰性稀释剂E为聚乙二醇 (PEG)、聚丙二醇(PPG)、正辛醇等热解温度低于树脂混合物D聚合后热解温度的无反应性聚合物中的一种或几种。所述光引发剂、分散剂和流平剂均为市售常用试剂。
具体的,所述预聚体B和单体C、光引发剂混合时,B优选为单官能度PUA,C优选PPTTA和HEMA,PUA、PPTTA、HEMA比例优选为3:4:3,B和C混合后得到光敏树脂D,光引发剂为混合光敏树脂D质量的1%~3%;惰性稀释剂E可以为PPG或正辛醇(实施例中用具体的化学名体现),D、E以体积比混合得到F,其中E占F的50%~70%。
具体的,陶瓷浆料G中粉体A的体积固含量为35%~45%。
具体的,所述打印坯体H可以在空气气氛下以15℃/min脱脂,坯体无裂纹。
具体的,所述种植体J结构如图1所示。
与现有技术相比,本发明具备下述有益效果:
本发明所用到的氮化硅粉体粒径为0.8~1.5μm,经过低速超长时间的球磨,可以对氮化硅颗粒进行整形,提高氮化硅颗粒的流动性,有利于降低氮化硅浆料的粘度;本发明的混合光敏树脂D中含有大量的预聚体,固化后适合形成交联网络,膜强度提高,更适用于陶瓷3D打印,且PPTTA的高官能度可以提高光固化反应活性,提高固化深度和速度;本发明提供的浆料配方,可以在打印固化后进行全流程的10℃的超快速脱脂,惰性稀释剂的大量添加,使得坯体H在300℃以下的低温区脱脂时,可以获得联通的孔隙网络,使其在600~700℃时得到的坯体I表面无裂纹,大大提高了生产效率,烧结后的陶瓷可获得高抗弯强度和高断裂韧性;本发明提供的种植体孔结构设计,底端的十字尖瓣设计可以植入初期的植体稳定性,直径方向的孔结构非线性梯度设计,可以保证力学性能的同时,提高骨整合性和结合强度。
附图说明
图1为氮化硅陶瓷种植体示意图:1、球形基台,2、梯度孔结构,3、实心圆柱,4、带孔十字尖瓣。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,以下将结合具体实施例对本发明涉及的各个方面进行详细说明。这些具体实施例仅用于举例说明本发明,并不限定本发明的保护范围和实质内容。
实施例1:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,100rpm低速球磨96小时,120℃干燥6h后过200目筛网,得到粉体A;
S2、将PUA、PPTTA、HEMA以3:4:3的质量比用均质机混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、聚丙二醇200(PPG200)以1:1的体积比用均质机混合,加入粉体质量2%的分散剂BYK110和流平剂BYK360P,搅拌机搅拌30min得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为20000厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以3℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将脱脂坯体I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J;
种植体J由球形基台1、梯度孔结构2、实心圆柱3、带孔十字尖瓣4组成,其中带孔十字尖瓣厚度为0.4~0.6mm,孔径为400μm,梯度孔结构为从表面到中心的TPMS孔隙率梯度变化依次减小的结构,下述实施例如无特殊说明,种植体结构同实施例1。
实施例2:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,100rpm低速球磨126小时,120℃干燥6h后过200目筛网,得到粉体A;
S2、将PUA、PPTTA以3:7的质量比用均质机混合,添加1wt%的光引发剂819得到混合光敏树脂D;
S3、将D、聚丙二醇200(PPG200)以1:1的体积比用均质机混合,加入粉体质量2%的分散剂BYK163得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为26500厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以5℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例3:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以4:1的比例混合,200rpm低速球磨96小时,120℃干燥6h后过200目筛网,得到粉体A;
S2、将PUA、PPTTA、HEMA以3:4:3的质量比用均质机混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、正辛醇以1:1的体积比用均质机混合,加入粉体质量2%的分散剂BYK110和流平剂BYK360P得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为24800厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以3℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例4:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,200rpm低速球磨126小时,120℃干燥6h后过200目筛网,得到粉体A;
S2、将PUA、PPTTA以3:7的质量比用均质机混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、聚丙二醇200(PPG200)以1:1的体积比用均质机混合,加入粉体质量2%的分散剂Solsperse85000得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为23600厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以5℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例5:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以4:1的比例混合,100rpm低速球磨96小时,120℃干燥6h后过200目筛网,得到粉体A;
S2、将PUA、PPTTA、HEMA以3:4:3的质量比用均质机混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、正辛醇以1:1的体积比用均质机混合,加入粉体质量2%的BYK110和流平剂BYK360P得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为20500厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以5℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例6:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以4:1的比例混合,100rpm低速球磨96小时,然后干燥过200目筛网,得到粉体A;
S2、将PUA、PPTTA以3:7的质量比用均质机混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、正辛醇、PPG200以2:1:1的体积比用均质机混合,加入粉体质量2%的分散剂BYK110和流平剂BYK360P得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为17500厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以15℃/min的升温速率升温至200℃保温2h,以15℃/min的升温速率升温至300℃并保温1h,以15℃/min的升温速率升温至400℃并保温1h,以15℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例7:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以5:1的比例混合,100rpm低速球磨96小时,然后干燥过200目筛网,得到粉体A;
S2、将PUA、PPTTA以3:7的质量比均匀混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、正辛醇以1:1的体积比混合,加入粉体质量2%的分散剂BYK110和流平剂BYK360P得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为17500厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以5℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间无开裂;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
实施例8:
本发明提供一种3D打印氮化硅陶瓷种植体,具体制备过程包括:
S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以5:1的比例混合,100rpm低速球磨96小时,然后干燥过200目筛网,得到粉体A;
S2、将PUA、PPTTA、HEMA以3:4:3的质量比均匀混合,添加2wt%的光引发剂819得到混合光敏树脂D;
S3、将D、PPG200以1:1的体积比混合,加入粉体质量2%的分散剂BYK110和流平剂BYK360P得到光敏树脂F;
S4、将A和F均匀混合后得到固含量为45%的陶瓷浆料G,浆料粘度为17000厘泊;
S5、将G利用光固化设备进行3D打印成型得到打印坯体H;
S6、将H以3℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I,脱脂后坯体表面无裂纹,层间有轻微分层;
S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到如图1所示的陶瓷种植体J。
对比例1:
详细制备过程和实施例1相同,其区别为:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,350rpm高速球磨24小时,然后干燥过200目筛网,得到粉体A。
对比例2:
详细制备过程和实施例1相同,其区别为:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,350rpm高速球磨200小时,然后干燥过200目筛网,得到粉体A。
对比例3:
详细制备过程和实施例1相同,其区别为:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,50rpm球磨24小时,然后干燥过200目筛网,得到粉体A。
对比例4:
详细制备过程和实施例1相同,其区别为:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1的比例混合,50rpm球磨200小时,然后干燥过200目筛网,得到粉体A。
对比例5:
详细制备过程和实施例2相同,其区别为:S3、将D、聚丙二醇200(PPG200)以3:1的体积比混合,加入粉体质量2%的分散剂和流平剂得到光敏树脂F。
对比例6:
详细制备过程和实施例2相同,其区别为:S3、将D、聚丙二醇200(PPG200)以2:1的体积比混合,加入粉体质量2%的分散剂和流平剂得到光敏树脂F。
对比例7:
详细制备过程和实施例2相同,其区别为: S6、将H以15℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体。
对比例8:
详细制备过程和实施例3相同,其区别为: S6、将H以10℃/min的升温速率升温至200℃保温2h,以10℃/min的升温速率升温至300℃并保温1h,以10℃/min的升温速率升温至400℃并保温1h,以10℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I。
对比例9:
详细制备过程和实施例6相同,其区别为得到光敏树脂F的工艺不同:将PUA、PPTTA以3:7的质量比称取,再将正辛醇、PPG200以总体积的50%比例加入PUA和PPTTA中,加入光引发剂,加入粉体质量2%的分散剂Solsperse85000,均质机混合后得到光敏树脂F。
对比例10:
详细制备过程和实施例6相同,其区别为:S3、将D、正辛醇、PPG200以1:1:1的体积比用均质机混合,加入粉体质量2%的分散剂Solsperse85000和流平剂BYK360P得到光敏树脂F。
不同工艺下所获得的性能主要表现在浆料粘度、脱脂效果上,区别见表1:
表1
实施例 | 浆料粘度(厘泊) | 脱脂效果 |
实施例1 | 20000 | 坯体表面无裂纹,层间无开裂 |
实施例2 | 26500 | 坯体表面无裂纹,层间无开裂 |
实施例3 | 24800 | 坯体表面无裂纹,层间无开裂 |
实施例4 | 23600 | 坯体表面无裂纹,层间无开裂 |
实施例5 | 20500 | 坯体表面无裂纹,层间无开裂 |
实施例6 | 19500 | 坯体表面无裂纹,层间无开裂 |
实施例7 | 17500 | 坯体表面无裂纹,层间无开裂 |
实施例8 | 18800 | 坯体表面无裂纹,层间无开裂 |
对比例1 | 38400 | 坯体表面无裂纹,层间无开裂 |
对比例2 | 34550 | 坯体表面无裂纹,层间无开裂 |
对比例3 | 37700 | 坯体表面无裂纹,层间无开裂 |
对比例4 | 35050 | 坯体表面无裂纹,层间无开裂 |
对比例5 | 46400 | 坯体表面无裂纹,层间轻微开裂 |
对比例6 | 37630 | 坯体表面无裂纹,层间轻微开裂 |
对比例7 | 26500 | 坯体表面无裂纹,层间轻微开裂 |
对比例8 | 24800 | 坯体表面无裂纹,层间轻微开裂 |
对比例9 | 31010 | 坯体表面轻微裂纹,层间轻微开裂 |
对比例10 | 20200 | 坯体表面无裂纹,层间无开裂 |
通过以上实施例和对比例可以得到,本发明通过调整工艺和配方,制备了较低粘度的浆料,以及700℃以下脱脂过程最高15℃/min 的升温速率,可得到如图1所示的复杂医用种植体,制备效率高。
本发明提供的陶瓷种植体,以口腔种植手术为例,在牙槽骨常规手术备洞后,洞底开一十字缝隙将带孔十字尖瓣4插入缝隙中,可以起到稳定种植体位置的作用,与骨组织形成有效周向锚固,种植体底部的带孔十字尖瓣厚度为0.4~0.6mm,孔径为400μm。梯度孔结构2由圆柱外侧向中心呈孔密度由大减小的趋势,实心圆柱3保证陶瓷种植体的力学性能,基台1用于和牙冠的粘接。
以上所述仅是本发明的优选实施方式,应当指出的是,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种氮化硅陶瓷种植体,其特征为种植体由球形基台、梯度孔结构、实心圆柱、带孔十字尖瓣组成,其中球形基台根部过渡直径小于球形基台直径,带孔十字尖瓣厚度为0.4~0.6mm,孔径为400μm。
2.一种如权利要求1所述的氮化硅陶瓷种植体的制备方法,其特征为经过以下步骤制成:S1、将氮化硅粉体和烧结助剂混合后球磨,研磨球和粉体质量比以3:1~5:1的比例混合,100~200rpm低速球磨96~126小时,干燥后过200目筛网,得到粉体A;S2、将预聚体B和单体C、光引发剂以一定质量比均匀混合得到混合光敏树脂D;S3、将D、惰性稀释剂E、分散剂、流平剂以一定体积比均匀混合后,得到光敏树脂F,其中惰性稀释剂E占F总体积的50%~70%;S4、将A和F以一定比例均匀混合后得到陶瓷浆料G;S5、将G利用光固化设备进行3D打印成型得到打印坯体H;S6、将H以3~15℃/min的升温速率在空气环境下进行升温并保温一段时间得到脱脂坯体I;S7、将I以10℃/min的升温速率升至1900℃,保温3h,随炉冷却,得到陶瓷种植体。
3.如权利要求2所述的氮化硅陶瓷种植体的制备方法,其特征为步骤S1优选为研磨球和粉体质量比以3:1的比例混合,100rpm低速球磨96小时。
4.如权利要求2所述的氮化硅陶瓷种植体的制备方法,其特征为步骤S3优选为惰性稀释剂E为正辛醇和PPG200体积比1:1,光敏树脂F中D、E的体积比为1:1。
5.如权利要求2所述的氮化硅陶瓷种植体的制备方法,其特征为步骤S6优选为将H以15℃/min的升温速率升温至200℃保温2h,以15℃/min的升温速率升温至300℃并保温1h,以15℃/min的升温速率升温至400℃并保温1h,以15℃/min的升温速率升温至700℃并保温1h,降温后得到脱脂坯体I。
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Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050079201A1 (en) * | 2003-05-28 | 2005-04-14 | Jorg Rathenow | Implants with functionalized carbon surfaces |
CN1791437A (zh) * | 2003-05-16 | 2006-06-21 | 布卢薄膜有限责任公司 | 具有生物相容性涂层的医用植入物 |
CN203425052U (zh) * | 2013-08-26 | 2014-02-12 | 南宁越洋科技有限公司 | 一种供教学和普及推广种牙的两用型种植体 |
CN105232169A (zh) * | 2015-10-16 | 2016-01-13 | 福建中科康钛材料科技有限公司 | 多段式种植体组件及其制备方法 |
CN107158474A (zh) * | 2017-05-26 | 2017-09-15 | 山东工业陶瓷研究设计院有限公司 | 光固化3d打印牙科种植体用浆料及其制备方法和应用 |
CN107773315A (zh) * | 2017-11-10 | 2018-03-09 | 山东工业陶瓷研究设计院有限公司 | 一种连接陶瓷部件的连接结构及牙种植体 |
CN210541885U (zh) * | 2019-05-29 | 2020-05-19 | 陕西科技大学 | 一种牙齿种植体 |
CN112516381A (zh) * | 2020-12-28 | 2021-03-19 | 杭州而然科技有限公司 | 晶须补强氧化锆种植体 |
CN213697282U (zh) * | 2020-10-26 | 2021-07-16 | 武汉大学 | 一种用于固定软组织游离瓣的种植体愈合基台 |
CN114105650A (zh) * | 2022-01-26 | 2022-03-01 | 中国人民解放军国防科技大学 | 下沉式dlp光固化技术3d打印制备氮化硅陶瓷的方法 |
CN114524676A (zh) * | 2022-02-25 | 2022-05-24 | 广东工业大学 | 一种光固化氮化硅陶瓷浆料、氮化硅陶瓷的制备方法 |
-
2023
- 2023-10-17 CN CN202311338390.9A patent/CN117064579B/zh active Active
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1791437A (zh) * | 2003-05-16 | 2006-06-21 | 布卢薄膜有限责任公司 | 具有生物相容性涂层的医用植入物 |
US20050079201A1 (en) * | 2003-05-28 | 2005-04-14 | Jorg Rathenow | Implants with functionalized carbon surfaces |
CN203425052U (zh) * | 2013-08-26 | 2014-02-12 | 南宁越洋科技有限公司 | 一种供教学和普及推广种牙的两用型种植体 |
CN105232169A (zh) * | 2015-10-16 | 2016-01-13 | 福建中科康钛材料科技有限公司 | 多段式种植体组件及其制备方法 |
CN107158474A (zh) * | 2017-05-26 | 2017-09-15 | 山东工业陶瓷研究设计院有限公司 | 光固化3d打印牙科种植体用浆料及其制备方法和应用 |
CN107773315A (zh) * | 2017-11-10 | 2018-03-09 | 山东工业陶瓷研究设计院有限公司 | 一种连接陶瓷部件的连接结构及牙种植体 |
CN210541885U (zh) * | 2019-05-29 | 2020-05-19 | 陕西科技大学 | 一种牙齿种植体 |
CN213697282U (zh) * | 2020-10-26 | 2021-07-16 | 武汉大学 | 一种用于固定软组织游离瓣的种植体愈合基台 |
CN112516381A (zh) * | 2020-12-28 | 2021-03-19 | 杭州而然科技有限公司 | 晶须补强氧化锆种植体 |
CN114105650A (zh) * | 2022-01-26 | 2022-03-01 | 中国人民解放军国防科技大学 | 下沉式dlp光固化技术3d打印制备氮化硅陶瓷的方法 |
CN114524676A (zh) * | 2022-02-25 | 2022-05-24 | 广东工业大学 | 一种光固化氮化硅陶瓷浆料、氮化硅陶瓷的制备方法 |
Non-Patent Citations (1)
Title |
---|
冯学鹏;蒋晓菡;夏德勇;盛扬;姜彦;张嵘;: "可降解聚氨酯丙烯酸酯生物材料的制备及其表征", 高分子学报, no. 10 * |
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