CN117510203A - 氧化锆陶瓷假体的制备工艺 - Google Patents

氧化锆陶瓷假体的制备工艺 Download PDF

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CN117510203A
CN117510203A CN202311480150.2A CN202311480150A CN117510203A CN 117510203 A CN117510203 A CN 117510203A CN 202311480150 A CN202311480150 A CN 202311480150A CN 117510203 A CN117510203 A CN 117510203A
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zirconia ceramic
zirconia
sintering
green body
stabilizer
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张云龙
曹玉超
吴梦飞
李志敏
张纪锋
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Beijing Ansong Technology Co ltd
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Abstract

本发明氧化锆陶瓷假体的制备工艺涉及一种陶瓷结构加工工艺。其目的是为了提供一种能够产出性能优异的氧化锆陶瓷假体的制备工艺。本发明氧化锆陶瓷假体的制备工艺包括以下步骤：S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.01～0.15wt％，烧结助剂的加入量为0.2～0.5wt％；S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；S30，将微粒置于模具中，在200～400MPa下冷压成型，得到生坯；S35，将生坯烘干；S40，将生坯在750～1200℃保温，完成预烧，得到素坯；S50，将素坯空气气氛或真空气氛的烧结炉中，在1300～1500℃烧结1～5小时，得到产品。

Description

氧化锆陶瓷假体的制备工艺
技术领域
本发明涉及陶瓷技术领域，特别是涉及一种氧化锆陶瓷假体的制备工艺。
背景技术
采用人工假体来替换受损的关节已经成为临床上治疗关节疾病的首要选择。目前，临床上用来替换受损髋关节或膝关节的人工假体有金属对聚乙烯型、金属对金属型、陶瓷对聚乙烯型和陶瓷对陶瓷型。其中，陶瓷对聚乙烯型和陶瓷对陶瓷型由于显著降低的磨损量而得到越来越普通的应用。
陶瓷材料主要是氧化铝陶瓷、氧化锆陶瓷和氧化铝-氧化锆复合陶瓷。其中氧化锆(ZrO2)化学性质不活泼，具有高熔点、高折射率、低热膨胀系数和优异的生物相容性等特性，广泛应用于耐火材料、结构陶瓷、生物陶瓷以及电子功能陶瓷等领域。
现有技术多采用共沉淀法或者溶胶凝胶法制备部分稳定氧化锆粉末，该方法存在如下缺点：二次成型，其中首次成型为单向压力压制成型，压力为20～100MPa，该成型过程易造成生坯不均匀且形成硬度较高的二次颗粒，该二次颗粒在二次成型(成型压力为200～280MPa)过程中空气不易排出，影响最终性能。
发明内容
本发明要解决的技术问题是提供一种能够产出性能优异的氧化锆陶瓷假体的制备工艺。
本发明氧化锆陶瓷假体的制备工艺，包括以下步骤：
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.01～0.15wt％，烧结助剂的加入量为0.2～0.5wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在200～400MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在750～1200℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1300～1500℃烧结1～5小时，得到产品。
本发明氧化锆陶瓷假体的制备工艺，其中步骤S10中的稳定剂为氧化钇或氧化镱中的一种或两种。
本发明氧化锆陶瓷假体的制备工艺，其中步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。
本发明氧化锆陶瓷假体的制备工艺，其中所述烧结助剂以氧化锆陶瓷的重量为基准，三氧化二钪和三氧化二镓的加入量为0.1～0.25wt％三氧化二钪、0.1～0.25wt％三氧化二镓。
本发明氧化锆陶瓷假体的制备工艺，其中步骤S20中的溶剂为水或乙醇。
本发明氧化锆陶瓷假体的制备工艺与现有技术不同之处在于，本发明氧化锆陶瓷假体的制备工艺解决了传统烧结技术导致的陶瓷性能不佳的问题，而且工艺本身流程简单，生产效率更高；进一步提高了氧化锆陶瓷骨植入假体的多方面性能，包括晶粒尺寸、致密度、抗弯强度、断裂韧性和抗水热老化性能等。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1
本发明氧化锆陶瓷假体的制备工艺包括以下步骤：
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.01wt％，烧结助剂的加入量为0.2wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在200MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在750℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1300℃烧结1小时，得到产品；
步骤S10中的稳定剂为氧化钇。
步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。以氧化锆陶瓷的重量为基准，烧结助剂三氧化二钪和三氧化二镓的加入量为0.1wt％三氧化二钪、0.1wt％三氧化二镓。
步骤S20中的溶剂为水。
实施例2
本发明氧化锆陶瓷假体的制备工艺包括以下步骤：
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.15wt％，烧结助剂的加入量为0.5wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在400MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在1200℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1500℃烧结5小时，得到产品；
步骤S10中的稳定剂为氧化镱。
步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。以氧化锆陶瓷的重量为基准，烧结助剂三氧化二钪和三氧化二镓的加入量为0.25wt％三氧化二钪、0.25wt％三氧化二镓。
步骤S20中的溶剂为乙醇。
实施例3
本发明氧化锆陶瓷假体的制备工艺包括以下步骤：
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.05wt％，烧结助剂的加入量为0.3wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在250MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在900℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1350℃烧结2小时，得到产品；
步骤S10中的稳定剂为氧化钇和氧化镱。
步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。以氧化锆陶瓷的重量为基准，烧结助剂三氧化二钪和三氧化二镓的加入量为0.15wt％三氧化二钪、0.15wt％三氧化二镓。
步骤S20中的溶剂为甲醇。
实施例4
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.1wt％，烧结助剂的加入量为0.4wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在300MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在1000℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1400℃烧结3小时，得到产品；
步骤S10中的稳定剂为氧化钇。
步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。以氧化锆陶瓷的重量为基准，烧结助剂三氧化二钪和三氧化二镓的加入量为0.2wt％三氧化二钪、0.2wt％三氧化二镓。
步骤S20中的溶剂为水。
实施例5
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.13wt％，烧结助剂的加入量为0.45wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在350MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在1100℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1450℃烧结4小时，得到产品；
步骤S10中的稳定剂为氧化镱。
步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。以氧化锆陶瓷的重量为基准，烧结助剂三氧化二钪和三氧化二镓的加入量为0.23wt％三氧化二钪、0.22wt％三氧化二镓。
步骤S20中的溶剂为乙醇。
对比例1
本对比例与实施例5的区别在于：没有加入烧结助剂。
以上实施例得到的氧化锆陶瓷骨植入假体的性能如表1所示。
表1氧化锆陶瓷骨植入假体的性能
由表1可确定，本发明所制备的氧化锆陶瓷假体体积密度≥6.10g/cm3，晶粒尺寸≤0.35μm，四点抗弯强度≥1145MPa，断裂韧性≥8.6MPa·m0.5；134℃水热处理5h后，表面单斜相含量≤1.03％，四点抗弯强度≥955MPa且保持率≥90％。本发明还测试了最终产品中氧化锆的纯度为ZrO2+HfO2≥90wt％，表面无单斜相。比较实施例5和对比例1可确定，加入烧结助剂更利于改善陶瓷的性能。
虽然，上文中已经用一般性说明及具体实施例对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (5)

1.一种氧化锆陶瓷假体的制备工艺，其特征在于：包括以下步骤：
S10，将氧化锆粉、稳定剂和烧结助剂混合研磨，得到浆料；以氧化锆粉的重量为基准，稳定剂的加入量为0.01～0.15wt％，烧结助剂的加入量为0.2～0.5wt％；
S20，向浆料中加入溶剂，混匀，喷雾干燥，得到微粒；
S30，将微粒置于模具中，在200～400MPa下冷压成型，得到生坯；
S35，将生坯烘干；
S40，将生坯在750～1200℃保温，完成预烧，得到素坯；
S50，将素坯空气气氛或真空气氛的烧结炉中，在1300～1500℃烧结1～5小时，得到产品。
2.根据权利要求1所述的氧化锆陶瓷假体的制备工艺，其特征在于：步骤S10中的稳定剂为氧化钇或氧化镱中的一种或两种。
3.根据权利要求1所述的氧化锆陶瓷假体的制备工艺，其特征在于：步骤S10中的烧结助剂为三氧化二钪和三氧化二镓中的组合物。
4.根据权利要求3所述的氧化锆陶瓷假体的制备工艺，其特征在于：所述烧结助剂以氧化锆陶瓷的重量为基准，三氧化二钪和三氧化二镓的加入量为0.1～0.25wt％三氧化二钪、0.1～0.25wt％三氧化二镓。
5.根据权利要求1所述的氧化锆陶瓷假体的制备工艺，其特征在于：步骤S20中的溶剂为水或乙醇。
CN202311480150.2A 2023-11-08 2023-11-08 氧化锆陶瓷假体的制备工艺 Pending CN117510203A (zh)

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