CN112250438B - 一种高均匀性全瓷义齿用氧化锆瓷块的制备方法及其制品 - Google Patents
一种高均匀性全瓷义齿用氧化锆瓷块的制备方法及其制品 Download PDFInfo
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Abstract
本发明公开了一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,以球形粉体颗粒为原料,所述粉体由氧化锆基料和外加物丙烯酸树脂组成,首先注入模具腔体进行干压,得到干压坯体后,放入温等静压机腔体中进行温压,然后再进行震荡冷压,即得到高均匀性全瓷义齿用氧化锆瓷块。此外还公开了利用上述高均匀性全瓷义齿用氧化锆瓷块的制备方法得到的制品。本发明所得制品均匀性高、强度稳定、加工缺陷少,有利于促进氧化锆在口腔修复领域的发展和应用。
Description
技术领域
本发明涉及齿科修复材料技术领域,尤其涉及一种高均匀性全瓷义齿用氧化锆瓷块的制备方法及其制品。
背景技术
口腔修复是非常古老的医学门类,很早以前,人们便已掌握使用柔软的贵金属作为口腔修复材料的技术。随着工业革命带来的理论技术逐步实用化,物美价廉的特种合金,如镍铬合金、钴铬合金、钛合金等逐渐替代贵金属,成为主流口腔修复材料。至此,口腔修复进入普及化和大众化阶段,极大提高了广大患者的生活质量。在满足功能需求的基础上,技术人员又开发出了金属烤瓷技术,通过物理仿真,实现了口腔修复材料的美学化提升。然而,令人始料未及的是,金属基义齿在长期使用后,会导致牙龈呈现乌黑色泽,其根本原因是金属离子的溶出着色,这严重影响了口腔修复的美学效果。因此,义齿修复材料的全瓷化得到技术人员的广泛重视,氧化铝全瓷、氧化锂全瓷、白榴石全瓷等技术方案不断涌现并推向市场。但是,上述全瓷材料的抗弯强度和断裂韧性普遍较低,难以完全胜任口腔复杂环境的力学要求。部分材料因自身折射率、着色性等物理特性所限,也无法实现高标准的美学需求。故而在很长一段时间里,金属烤瓷和氧化物全瓷在口腔修复领域呈现胶着共存的状态。直到本世纪初,因纳米技术的发展,具有优异力学性能、出众美学效果以及良好生物相容性的氧化锆开始步入实用阶段,逐步替代氧化物、合金等材料在口腔修复领域的使用。
现有技术制备氧化锆瓷块,首先是将纳米氧化锆制成球形颗粒,然后填充模具压制成型,使之具备一定的密度(一般是3.0~3.2g/cm3),再通过热处理(900~1100℃)使之具备一定的加工强度。义齿技工利用这种瓷块在CAD/CAM技术辅助下,通过切削加工设备制作所需形状的修复体生坯,经烧结成瓷,制得氧化锆全瓷修复体,根据定制要求进行美学修饰后供医生使用。这种瓷块是由纳米氧化锆团聚体堆砌而成,其均匀度相比锻造成型的合金材料有很大不足,球形颗粒的均匀度变化以及压制成型的均匀度不佳进一步放大了这种缺陷,导致氧化锆材料的强度波动很大,可靠性不足,仅在三单位以下的修复需求下有较大把握,长桥和半口的返工率偏高,种植体更是禁区。同时,加工修复体生坯过程中,瓷块的均匀度会影响表面光洁度,进而降低修复体的美学效果,增加饰瓷工作量,上述这些因素很大程度影响了氧化锆的进一步规模化应用。
发明内容
本发明的目的在于克服现有技术的不足,提供一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,以获得均匀性高、强度稳定、加工缺陷少的氧化锆修复体,促进氧化锆在口腔修复领域的发展和应用。本发明另一目的在于提供利用上述制备方法得到的制品。
本发明的目的通过以下技术方案予以实现:
本发明提供的一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,包括以下步骤:
(1)将球形粉体颗粒注入模具腔体进行干压,得到干压坯体;所述粉体由氧化锆基料和外加物组成;所述氧化锆基料的组成为氧化锆90~96wt%、添加物4~10wt%,其中添加物为氧化钇、氧化铒、氧化镨、氧化钕、氧化钴、氧化锰、氧化铁、氧化铈、氧化镧、氧化镱、氧化镓中的一种或其组合;所述外加物为丙烯酸树脂,其用量为氧化锆基料的2~10wt%;
(2)所述干压坯体经真空包装后,放入温等静压机腔体中进行温压,得到温压坯体;
(3)将所述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,即得到高均匀性全瓷义齿用氧化锆瓷块。
上述方案中,本发明所述丙烯酸树脂的Tg(玻璃化转变温度)为-30℃≤Tg≤+60℃;所述粉体中含有两种或两种以上不同Tg的丙烯酸树脂。
进一步地,本发明所述粉体的平均团聚尺寸为0.1~0.5μm。所述步骤(2)中的温压参数为温度80~90℃,压力90~120MPa。所述步骤(3)中震荡冷压的升压速率为2MPa/s,最高压力为250~300MPa,高压保压时间为300~900s,高压震荡幅度为10~50MPa,震荡频率为0.2~50Hz。
利用上述高均匀性全瓷义齿用氧化锆瓷块的制备方法得到的制品,其各区域的密度差异≤0.05g/cm3,韦伯模数≥12.2。
本发明具有以下有益效果:
(1)本发明在不增加球形粉体颗粒硬度的情况下,通过采用不同Tg的丙烯酸树脂,可极大提高其流动性和塑性,从而有利于极大地提高模具填充均匀度,配合温等静压处理,可减少颗粒间的微观气孔。
(2)本发明通过采用震荡冷压,对成型过程中的孔隙缺陷进一步修复,减少了气孔平均尺寸,有效提高了瓷块均匀度,避免对强度分布造成影响,所得制品均匀性高、强度稳定、加工缺陷少,有利于促进氧化锆在口腔修复领域的发展和应用。
下面将结合实施例对本发明作进一步的详细描述。
具体实施方式
实施例一:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.3μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆96wt%、氧化铒4wt%;外加物为Tg=-30℃和Tg=60℃的两种丙烯酸树脂,其用量为氧化锆基料的5wt%,其中按照质量比丙烯酸树脂(Tg=-30℃)∶丙烯酸树脂(Tg=60℃)=2∶3;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为80℃,压力为100MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为290MPa,保压时间为600s,震荡幅度为20MPa,震荡频率为30Hz,即得到密度均匀(各区域密度差异小于0.03g/cm3)、烧结体抗弯强度离散小(韦伯模数为13.5)的全瓷义齿用氧化锆瓷块。
实施例二:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.5μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆94.6wt%、氧化钇5wt%、氧化铁0.1wt%、氧化镓0.3wt%;外加物为Tg=-30℃、Tg=40℃和Tg=60℃的三种丙烯酸树脂,其用量为氧化锆基料的2wt%,其中按照质量比丙烯酸树脂(Tg=-30℃)∶丙烯酸树脂(Tg=40℃)∶丙烯酸树脂(Tg=60℃)=1∶1∶3;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为85℃,压力为110MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为250MPa,保压时间为800s,震荡幅度为25MPa,震荡频率为50Hz,即得到密度均匀(各区域密度差异小于0.05g/cm3)、烧结体抗弯强度离散小(韦伯模数为13.0)的全瓷义齿用氧化锆瓷块。
实施例三:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.4μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆90.87wt%、氧化钇7wt%、氧化钕0.01wt%、氧化镨0.1wt%、氧化钴0.05wt%、氧化锰0.02wt%、氧化铁0.15wt%、氧化铈0.3wt%、氧化镧0.5wt%、氧化镱1.0wt%、氧化镓0.1wt%;外加物为Tg=-20℃、Tg=0℃和Tg=40℃的三种丙烯酸树脂,其用量为氧化锆基料的8wt%,其中按照质量比丙烯酸树脂(Tg=-20℃)∶丙烯酸树脂(Tg=0℃)∶丙烯酸树脂(Tg=40℃)=1∶2∶7;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为90℃,压力为105MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为260MPa,保压时间为400s,震荡幅度为40MPa,震荡频率为5Hz,即得到密度均匀(各区域密度差异小于0.03g/cm3)、烧结体抗弯强度离散小(韦伯模数为13.9)的全瓷义齿用氧化锆瓷块。
实施例四:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.2μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆90wt%、氧化钇9.5wt%、氧化铈0.5wt%;外加物为Tg=20℃和Tg=60℃的两种丙烯酸树脂,其用量为氧化锆基料的4wt%,其中按照质量比丙烯酸树脂(Tg=20℃)∶丙烯酸树脂(Tg=60℃)=1∶1;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为88℃,压力为120MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为300MPa,保压时间为300s,震荡幅度为50MPa,震荡频率为0.5Hz,即得到密度均匀(各区域密度差异小于0.04g/cm3)、烧结体抗弯强度离散小(韦伯模数为12.2)的全瓷义齿用氧化锆瓷块。
实施例五:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.1μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆90.4wt%、氧化钇9wt%、氧化铁0.2wt%、氧化镨0.4wt%、氧化铈0.4wt%;外加物为Tg=-30℃、Tg=-10℃、Tg=20℃和Tg=60℃的四种丙烯酸树脂,其用量为氧化锆基料的的10wt%,其中按照质量比丙烯酸树脂(Tg=-30℃)∶丙烯酸树脂(Tg=-10℃)∶丙烯酸树脂(Tg=20℃)∶丙烯酸树脂(Tg=60℃)=5∶7∶15∶73;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为82℃,压力为90MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为250MPa,保压时间为500s,震荡幅度为10MPa,震荡频率为2Hz,即得到密度均匀(各区域密度差异小于0.02g/cm3)、烧结体抗弯强度离散小(韦伯模数为12.8)的全瓷义齿用氧化锆瓷块。
实施例六:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.3μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆93.18wt%、氧化钇6wt%、氧化钴0.01wt%、氧化钕0.01wt%、氧化镧0.8wt%;外加物为Tg=0℃和Tg=60℃的两种丙烯酸树脂,其用量为氧化锆基料的7wt%,其中按照质量比丙烯酸树脂(Tg=0℃)∶丙烯酸树脂(Tg=60℃)=7∶13;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为85℃,压力为95MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为270MPa,保压时间为700s,震荡幅度为45MPa,震荡频率为0.2Hz,即得到密度均匀(各区域密度差异小于0.04g/cm3)、烧结体抗弯强度离散小(韦伯模数为15.1)的全瓷义齿用氧化锆瓷块。
实施例七:
本实施例一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其步骤如下:
(1)将平均团聚尺寸为0.4μm的球形粉体颗粒注入模具腔体进行干压,得到干压坯体;粉体由氧化锆基料和外加物组成,其中,氧化锆基料的组成为氧化锆95.4wt%、氧化钇4wt%、氧化锰0.1wt%、氧化镱0.5wt%;外加物为Tg=-25℃和Tg=55℃的两种丙烯酸树脂,其用量为氧化锆基料的6wt%,其中按照质量比丙烯酸树脂(Tg=-25℃)∶丙烯酸树脂(Tg=55℃)=11∶9;
(2)上述干压坯体经真空包装后,放入温等静压机腔体中进行温压,温等静压温度为80℃,压力为115MPa,得到温压坯体;
(3)将上述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,震荡冷压的升压速率为2MPa/s,最高压力为260MPa,保压时间为900s,震荡幅度为35MPa,震荡频率为25Hz,即得到密度均匀(各区域密度差异小于0.05g/cm3)、烧结体抗弯强度离散小(韦伯模数为14.5)的全瓷义齿用氧化锆瓷块。
Claims (5)
1.一种高均匀性全瓷义齿用氧化锆瓷块的制备方法,其特征在于包括以下步骤:
(1) 将球形粉体颗粒注入模具腔体进行干压,得到干压坯体;所述粉体由氧化锆基料和外加物组成;所述氧化锆基料的组成为氧化锆90~96 wt%、添加物4~10 wt%,其中添加物为氧化钇、氧化铒、氧化镨、氧化钕、氧化钴、氧化锰、氧化铁、氧化铈、氧化镧、氧化镱、氧化镓中的一种或其组合;所述外加物为Tg为-30 oC≤Tg≤60oC的丙烯酸树脂,其用量为氧化锆基料的2~10 wt%;所述粉体中含有两种或两种以上不同Tg的丙烯酸树脂;
(2) 所述干压坯体经真空包装后,放入温等静压机腔体中进行温压,得到温压坯体;
(3) 将所述温压坯体更换真空包装,放入冷等静压机腔体中进行震荡冷压,升压速率为2 MPa/s,最高压力为250~300 MPa,高压保压时间为300~900 s,高压震荡幅度为10~50 MPa,震荡频率为0.2~50 Hz,即得到高均匀性全瓷义齿用氧化锆瓷块。
2.根据权利要求1所述的高均匀性全瓷义齿用氧化锆瓷块的制备方法,其特征在于:所述粉体的平均团聚尺寸为0.1~0.5 μm。
3.根据权利要求1所述的高均匀性全瓷义齿用氧化锆瓷块的制备方法,其特征在于:所述步骤(2)中的温压参数为温度80~90 oC,压力90~120 MPa。
4.利用权利要求1-3之一所述高均匀性全瓷义齿用氧化锆瓷块的制备方法得到的制品。
5.根据权利要求4所述的高均匀性全瓷义齿用氧化锆瓷块的制备方法得到的制品,其特征在于:所述氧化锆瓷块制品各区域的密度差异≤0.05 g/cm3,韦伯模数≥12.2。
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