CN110078500A - 一种牙科氧化锆全瓷材料及其制备方法 - Google Patents

一种牙科氧化锆全瓷材料及其制备方法 Download PDF

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CN110078500A
CN110078500A CN201910508840.1A CN201910508840A CN110078500A CN 110078500 A CN110078500 A CN 110078500A CN 201910508840 A CN201910508840 A CN 201910508840A CN 110078500 A CN110078500 A CN 110078500A
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zirconium oxide
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孔令兵
张天舒
刘银
董强
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Nanjing Sanotes Material Technology Co Ltd
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Abstract

本发明涉及一种牙科氧化锆全瓷材料的制备方法,所述牙科氧化锆全瓷材料是通过以下制备方法来制备的:按照一定比例精确称取用于制备所述牙科氧化锆全瓷材料的原料:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂;将所述陶瓷粉料、稳定剂以及至少部分助剂在存在一定量溶剂或无溶剂条件下进行混合球磨或砂磨,得到物料粉体,将所述造孔剂、粘结剂以及其余部分助剂分别在加热或冷却的条件下加入所述物料粉体中,得到物料悬浮液并将其置于模具中冷却干燥,得到所述牙科氧化锆全瓷材料。

Description

一种牙科氧化锆全瓷材料及其制备方法
技术领域
本发明涉及牙科材料技术领域,尤其涉及一种牙科氧化锆全瓷材料及其制备方法。
背景技术
全瓷修复技术因具有良好的生物相容性和优越的美观效果,成为口腔材料的较为理想的选择,在全瓷材料系统中,氧化锆陶瓷的强度、韧性等机械性能明显优于其他材料,是目前口腔材料关注和研究的焦点,它在氧化物陶瓷中占有重要地位。氧化锆陶瓷材料能够解决常规全瓷材料强度和韧性不足等问题,并且它属于生物惰性陶瓷类材料,在生物医学领域得到了广泛应用。
氧化锆生物陶瓷由高纯二氧化锆构成的一种近于惰性的生物陶瓷,其是通过将含有少量稳定剂的高纯二氧化锆经过高温烧结而制得,高稳定剂例如为氧化钙、氧化镁或氧化钇。不仅具有良好的耐磨性、抗生理腐蚀性和生物相容性,而且其断裂韧性性和强度均优于氧化铝陶瓷。主要用于人体关节、牙种植体等硬组织的修复和替换。
氧化锆具有极高的化学稳定性和热稳定性,其Tm=2953K,在生理环境中呈现惰性,具有很好的生物相容性。纯氧化锆具有三种同素异型体:单斜氧化锆(m相)、四方氧化锆(t相)以及立方氧化锆(c相),三种同素异型体存在于不同的温度范围,并在一定条件下可以发生晶型转化(相变)。氧化锆通常室温下仅以单斜相形式存在,但加入适量有利于稳定四方相的SrO、MgO、Y2O3、CaO、Sc2O3、La2O3及Mn2O3等氧化物与氧化锆之间形成固溶体,可以使得氧化锆的四方以及立方晶型在室温下仍保持稳定或亚稳态。通过应力诱导相变增韧使氧化锆陶瓷具有很高的力学性能。在承受外力作用时,其四方氧化锆(t相)向单斜氧化锆(m相)转化的过程需吸收较高的能量,使裂纹尖端应力松弛,增加裂纹扩散阻力而增韧,因而具有非常高的断裂韧性。部分稳定的氧化锆和氧化铝一样,生物相容性良好,在人体内稳定性高,且比氧化铝断裂韧性、耐磨性更高,有利减少植入物尺寸和实现低摩擦、磨损,用以制造牙根、骨、股关节、复合陶瓷人工骨、瓣膜等。
虽然氧化锆陶瓷具有优秀的力学性能,但其作为生物惰性材料却不能与骨组织形成化学结合,影响植入体的可靠性和长期疗效。现有技术中往往通过加入生物活性成分或表面改性的方法,使得氧化锆陶瓷具有一定的生物活性,要求其能够达到赋予氧化锆陶瓷生物活性的同时不会对其力学性能产生明显的影响,并且生物活性表面层的接合强度以及长期稳定性要能够满足临床应用的要求。
牙科常用的氧化锆陶瓷包括:四方相氧化锆陶瓷、氧化锆增韧陶瓷、部分稳定氧化锆陶瓷及纳米氧化锆与氧化铝复合陶瓷,这四种氧化锆陶瓷都含有稳定的四方相,并通过其四方氧化锆(t相)向单斜氧化锆(m相)的马氏体相变增韧,但微观结构各不相同,决定了不同的性能和加工工艺。
中国专利(公开号为CN107827457A)公开了一种多孔氧化锆陶瓷的制备方法,先将氧化锆和氧化钇按重量配比混合均匀制备混合料;然后制备聚丙烯醇水溶液和氯化铵水溶液:将所得混合料和溶液一起放入球磨机中进行球磨;向球磨后的浆料中加入粘结剂、淀粉溶液、表面活性剂,继续球磨30min;之后加入10%的氯化铵水溶液,高速下球磨3min,迅速倒入模具中成型;将模具和模具中的浆料放入烘箱中进行发泡;然后放入冷冻箱中冷冻,形成凝胶;将凝胶样品进行脱模,经干燥后烧结,得到多孔氧化锆陶瓷。本发明用磷酸锌作为粘结剂,提高了粘结强度,降低了污染,得到的多孔氧化锆陶瓷孔隙率高,孔径均匀,提高了多孔氧化锆陶瓷的性能。
然而上述专利并未消除现有技术中氧化锆晶粒的粒径大小对所制备的全瓷材料造成的影响:由于在氧化锆的粒径过大的情况下容易造成氧化锆晶粒的生长尺寸过大,使得其力学性能较差;而在氧化锆的粒径过小的情况下,氧化锆粉体之间容易发生团聚现象而保持有气泡,将导致脱模成型后的产品存在内部缺陷,使其力学性能较差。
此外,一方面由于对本领域技术人员的理解存在差异;另一方面由于发明人做出本发明时研究了大量文献和专利,但篇幅所限并未详细罗列所有的细节与内容,然而这绝非本发明不具备这些现有技术的特征,相反本发明已经具备现有技术的所有特征,而且申请人保留在背景技术中增加相关现有技术之权利。
发明内容
针对现有技术之不足,本发明提供了一种牙科氧化锆全瓷材料的制备方法,所述牙科氧化锆全瓷材料是通过以下制备方法来制备的:按照一定比例精确称取用于制备所述牙科氧化锆全瓷材料的原料:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂;将所述陶瓷粉料、稳定剂以及至少部分助剂在存在一定量溶剂或无溶剂条件下进行混合球磨或砂磨,得到物料粉体,将所述造孔剂、粘结剂以及其余部分助剂分别在加热或冷却的条件下加入所述物料粉体中,得到物料悬浮液并将其置于模具中冷却干燥,得到所述牙科氧化锆全瓷材料。
根据一种优选实施方式,所述造孔剂至少包括CaTiSiO5、(C6H10O5)n、(C10H14O4·C5H8O2)n、(C8H8)n中的一个或几个的组合。
根据一种优选实施方式,所述粘结剂至少包括[CH2CH]nCOOH、C35H49O29、C6H7O2(OH)2OCH2COONa、[CH2CHOH]n、[CH2CH2O]n中的一个或几个的组合。
根据一种优选实施方式,所述稳定剂至少包括SrO、Y2O3、Sc2O3、La2O3、MgO中的一个或几个的组合。
根据一种优选实施方式,所述助剂至少包括在进行混合球磨或砂磨时加入的分散剂,其中,所述分散剂至少包括C12H25NaO4S、C6H15O3N、CH3CH2OH、CH3(CH2)16COOH、C24H54O8P2、C6H14O、[C3H5NO]n中的一个或几个的组合。
根据一种优选实施方式,所述助剂至少包括用于加入所述物料粉体中进行对其上色的着色剂,其中,所述着色剂至少包括Fe2O3、Er2O3、Bi2O3、NiO、ZrSiO4、SiO2中的一个或几个的组合。
根据一种优选实施方式,所述陶瓷粉料至少包括摩尔含量为90~98%的ZrO2、摩尔含量为2~10%的Al2O3中的一个或几个的组合,所述溶剂至少包括去离子水或乙醇水溶液。
根据一种优选实施方式,所述助剂至少包括用于提高所述牙科氧化锆全瓷材料的抑菌效果的抑菌剂,其中,所述抑菌剂至少包括牛蒡萃取剂、杜仲萃取剂、忍冬萃取剂、红腺忍冬萃取剂中的一个或几个的组合。
根据一种优选实施方式,所述牙科氧化锆全瓷材料由如下组分组成:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂,其中,所述陶瓷粉料占所有组分原料的质量份数为45~75%,所述造孔剂占所有组分原料的质量份数为10~20%,所述粘结剂占所有组分原料的质量份数为6~12%,所述稳定剂占所有组分原料的质量份数为10~30%,所述助剂占所有组分原料的质量份数为5~20%,所述组分原料中各组分的质量份数之和为100%。
根据一种优选实施方式,所述助剂至少包括3~10%分散剂、0.5~5%着色剂、0.5~5%抑菌剂。
本发明提供的牙科氧化锆全瓷材料及其制备方法至少具有如下有益技术效果:
本发明提供的制备方法所得到的牙科氧化锆全瓷材料,通过添加稳定剂如SrO、Y2O3等与氧化锆晶体混合,有效地约束四方氧化锆(t相)转变至单斜氧化锆(m相)的转变过程,并通过添加陶瓷粉料如粒径在微米或亚微米级别的Al2O3等与氧化锆混合,有效地约束氧化锆晶粒的生长过程,结合稳定剂、陶瓷粉料以及造孔剂的作用叠加效应,有利于基于所述氧化锆所制备的物料悬浮液保持均匀稳定,有利于排出气泡而获得内部结构缺陷极少的脱模成型后的产品,且保证了脱模成型后的产品优异的力学性能与孔隙率,此外本发明提供的制备方法还通过添加抑菌剂保证所得到的牙科氧化锆全瓷材料的抑菌效果。
具体实施方式
本发明提供了一种牙科氧化锆全瓷材料的制备方法,所述牙科氧化锆全瓷材料是通过以下制备方法来制备的:将所述陶瓷粉料、稳定剂以及至少部分助剂在存在一定量溶剂或无溶剂条件下进行混合球磨或砂磨,得到物料粉体。将所述造孔剂、粘结剂以及其余部分助剂分别在加热或冷却的条件下加入所述物料粉体中,得到物料悬浮液。将物料悬浮液置于模具中冷却干燥,得到所述牙科氧化锆全瓷材料。现有技术中由于在氧化锆的粒径过大的情况下容易造成氧化锆晶粒的生长尺寸过大,使得其力学性能较差;而在氧化锆的粒径过小的情况下,氧化锆粉体之间容易发生团聚现象而保持有气泡,将导致脱模成型后的产品存在内部缺陷,使其力学性能较差。而本发明提供的制备方法所得到的牙科氧化锆全瓷材料,通过添加稳定剂如SrO、Y2O3等与氧化锆晶体混合,有效地约束四方氧化锆(t相)转变至单斜氧化锆(m相)的转变过程,并通过添加陶瓷粉料如粒径在微米或亚微米级别的Al2O3等与氧化锆混合,有效地约束氧化锆晶粒的生长过程,结合稳定剂、陶瓷粉料以及造孔剂的作用叠加效应,有利于基于所述氧化锆所制备的物料悬浮液保持均匀稳定,有利于排出气泡而获得内部结构缺陷极少的脱模成型后的产品,且保证了脱模成型后的产品优异的力学性能与孔隙率。
根据一种优选实施方式,造孔剂是指使材料中增加孔洞结构的添加剂,一般为易分解为气体的物质,本发明中所采用的造孔剂至少包括CaTiSiO5、(C6H10O5)n、(C10H14O4·C5H8O2)n、(C8H8)n、活性碳、纤维素甲醚中的一个或几个的组合。
根据一种优选实施方式,粘结剂是指为了提高压坯的强度或防止粉末偏析而添加到粉末中的可在烧结前或烧结过程中除掉的物质,本发明中所采用的粘结剂至少包括[CH2CH]nCOOH、C35H49O29、C6H7O2(OH)2OCH2COONa、[CH2CHOH]n、[CH2CH2O]n、乙烯吡咯烷酮聚合体或纤维素甲醚中的一个或几个的组合。
根据一种优选实施方式,常见的用于二氧化锆的稳定剂包括稀土或碱土氧化物,而且只有离子半径与Zr4+半径相差不超过40%的氧化物才能作为氧化锆的稳定剂目前稳定机理还不十分清楚。加入不同量的稳定剂可获得相组成不同的氧化锆陶瓷,若使部分t相ZrO2亚稳至室温,就得到部分稳定氧化锆;若使t相ZrO2全部亚稳至室温,获得仅含四方氧化锆的多晶体;若使c相ZrO2亚稳至室温,获得c相ZrO2单相材料,即全稳定氧化锆。部分稳定氧化锆和仅含四方氧化锆的多晶体中均含有可相变的四方相,是常用的相变增韧陶瓷。本发明中所采用的稳定剂至少包括SrO、Y2O3、Sc2O3、La2O3、MgO、CaO、Mn2O3中的一个或几个的组合。
根据一种优选实施方式,所述助剂至少包括在进行混合球磨或砂磨时加入的分散剂,分散剂是指在分子内同时具有亲油性和亲水性两种相反性质的界面活性剂,可均一分散那些难于溶解于液体的固体及液体颗粒,同时也能防止颗粒的沉降和凝聚。其中,本发明中所采用的分散剂至少包括C12H25NaO4S、C6H15O3N、CH3CH2OH、CH3(CH2)16COOH、C24H54O8P2、C6H14O、[C3H5NO]n、聚乙二醇月桂、纤维素及其衍生物中的一个或几个的组合。
根据一种优选实施方式,所述助剂至少包括用于加入所述物料粉体中进行对其上色的着色剂,着色剂即为在陶瓷上使用的颜料的通称,包括釉上、釉下以及釉料和坯体着色的陶瓷颜料,着色剂可以为粉末状的金属氧化物和其他用于陶瓷釉料中的混合物。其中,本发明中所采用的着色剂至少包括Fe2O3、Er2O3、Bi2O3、NiO、ZrSiO4、SiO2中的一个或几个的组合。
根据一种优选实施方式,所述陶瓷粉料至少包括二氧化锆、三氧化二铝、金属瓷粉、纯钛瓷粉、铸瓷粉中的一个或几个的组合,其中,二氧化锆的摩尔含量为90~98%、三氧化二铝的摩尔含量为2~10%。所述溶剂至少包括去离子水或乙醇水溶液。
根据一种优选实施方式,所述助剂至少包括用于提高所述牙科氧化锆全瓷材料的抑菌效果的抑菌剂,其中,所述抑菌剂至少包括牛蒡萃取剂、杜仲萃取剂、忍冬萃取剂、红腺忍冬萃取剂、毛花柱忍冬萃取剂、山银花萃取剂中的一个或几个的组合。
根据一种优选实施方式,所述牙科氧化锆全瓷材料由如下组分组成:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂,其中,所述陶瓷粉料占所有组分原料的质量份数为45~75%,所述造孔剂占所有组分原料的质量份数为10~20%,所述粘结剂占所有组分原料的质量份数为6~12%,所述稳定剂占所有组分原料的质量份数为10~30%,所述助剂占所有组分原料的质量份数为5~20%,所述组分原料中各组分的质量份数之和为100%。
根据一种优选实施方式,所述助剂至少包括按一定比例分开配置的分散剂、着色剂、抑菌剂。其中,分散剂的质量百分比为3~10%、着色剂的质量百分比为0.5~5%、抑菌剂的质量百分比为0.5~5%。本发明提供的制备方法还通过添加抑菌剂保证所得到的牙科氧化锆全瓷材料的抑菌效果。
需要注意的是,上述具体实施例是示例性的,本领域技术人员可以在本发明公开内容的启发下想出各种解决方案,而这些解决方案也都属于本发明的公开范围并落入本发明的保护范围之内。本领域技术人员应该明白,本发明说明书为说明性而并非构成对权利要求的限制。本发明的保护范围由权利要求及其等同物限定。

Claims (10)

1.一种牙科氧化锆全瓷材料的制备方法,其特征在于,用于制备所述牙科氧化锆全瓷材料的制备方法至少包括以下步骤:
按照一定比例称取用于制备所述牙科氧化锆全瓷材料的原料:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂,将所述陶瓷粉料、稳定剂以及至少部分助剂在存在一定量溶剂或无溶剂条件下进行混合球磨或砂磨,得到物料粉体,将所述造孔剂、粘结剂以及其余部分助剂分别在加热或冷却的条件下加入所述物料粉体中,得到物料悬浮液并将其置于模具中冷却干燥,得到所述牙科氧化锆全瓷材料。
2.根据权利要求1所述的制备方法,其特征在于,所述制备方法的造孔剂至少包括CaTiSiO5、(C6H10O5)n、(C10H14O4·C5H8O2)n、(C8H8)n中的一个或几个的组合。
3.根据前述权利要求之一所述的制备方法,其特征在于,所述制备方法的粘结剂至少包括[CH2CH]nCOOH、C35H49O29、C6H7O2(OH)2OCH2COONa、[CH2CHOH]n、[CH2CH2O]n中的一个或几个的组合。
4.根据前述权利要求之一所述的制备方法,其特征在于,所述制备方法的稳定剂至少包括SrO、Y2O3、Sc2O3、La2O3、MgO中的一个或几个的组合。
5.根据前述权利要求之一所述的制备方法,其特征在于,所述制备方法的助剂至少包括在进行混合球磨或砂磨时加入的分散剂,其中,所述分散剂至少包括C12H25NaO4S、C6H15O3N、CH3CH2OH、CH3(CH2)16COOH、C24H54O8P2、C6H14O、[C3H5NO]n中的一个或几个的组合。
6.根据前述权利要求之一所述的制备方法,其特征在于,所述制备方法的助剂至少包括用于加入所述物料粉体中进行对其上色的着色剂,其中,所述着色剂至少包括Fe2O3、Er2O3、Bi2O3、NiO、ZrSiO4、SiO2中的一个或几个的组合。
7.根据前述权利要求之一所述的制备方法,其特征在于,所述制备方法的陶瓷粉料至少包括摩尔含量为90~98%的ZrO2、摩尔含量为2~10%的Al2O3中的一个或几个的组合,所述溶剂至少包括去离子水或乙醇水溶液。
8.根据前述权利要求之一所述的制备方法,其特征在于,所述助剂至少包括用于提高所述牙科氧化锆全瓷材料的抑菌效果的抑菌剂,其中,所述抑菌剂至少包括牛蒡萃取剂、杜仲萃取剂、忍冬萃取剂、红腺忍冬萃取剂中的一个或几个的组合。
9.一种牙科氧化锆全瓷材料,其特征在于,所述牙科氧化锆全瓷材料由如下组分组成:陶瓷粉料、造孔剂、粘结剂、稳定剂、助剂,其中,所述陶瓷粉料占所有组分原料的质量份数为45~75%,所述造孔剂占所有组分原料的质量份数为10~20%,所述粘结剂占所有组分原料的质量份数为6~12%,所述稳定剂占所有组分原料的质量份数为10~30%,所述助剂占所有组分原料的质量份数为5~20%,所述组分原料中各组分的质量份数之和为100%。
10.根据权利要求9所述的牙科氧化锆全瓷材料,其特征在于,所述助剂至少包括3~10%分散剂、0.5~5%着色剂、0.5~5%抑菌剂。
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CN111704457A (zh) * 2020-07-24 2020-09-25 长沙博谱科学仪器有限公司 一种3d打印氧化锆基义齿材料及其制备方法
CN113693950A (zh) * 2021-09-17 2021-11-26 南京欧赛尔齿业有限公司 一种具有美白效果的前牙牙冠全瓷材料及其制备方法
CN113999007A (zh) * 2021-11-26 2022-02-01 上海陶宝陶瓷新材料开发有限公司 氧化锆多层色彩仿真陶瓷义齿生产工艺

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CN111704457A (zh) * 2020-07-24 2020-09-25 长沙博谱科学仪器有限公司 一种3d打印氧化锆基义齿材料及其制备方法
CN113693950A (zh) * 2021-09-17 2021-11-26 南京欧赛尔齿业有限公司 一种具有美白效果的前牙牙冠全瓷材料及其制备方法
CN113999007A (zh) * 2021-11-26 2022-02-01 上海陶宝陶瓷新材料开发有限公司 氧化锆多层色彩仿真陶瓷义齿生产工艺

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