CN108395246A - 一种高韧性口腔用纳米瓷粉材料的制备方法 - Google Patents
一种高韧性口腔用纳米瓷粉材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高韧性口腔用纳米瓷粉材料的制备方法，属于医用材料技术领域。本发明技术方案通过在陶瓷制备模具中沉积钼粉并经熔融包覆改性，通过三元金属硅化物Mo2SiZr的高硬度和金属键与原子键共存的原子间键合性质，使其在与其他金属零部件表面接触而发生摩擦磨损时难于发生金属黏着和变形，有效提高纳米瓷粉的耐磨性能和力学性能；且本发明采用纳米氧化锆改性复合瓷粉，由于采用与制备单相凝胶相同的方法，即改变溶液p值以得到两相混合液体的共同沉淀物，所制备的沉淀物材料具有优异的结合性能，有效提高本发明技术方案中氧化锆对材料的增韧改性程度，在一定程度上提高本发明技术方案的结合强度和力学性能。
Description
技术领域
本发明涉及一种高韧性口腔用纳米瓷粉材料的制备方法，属于医用材料技术领域。
背景技术
牙齿是人体的重要器官之一，有着十分重要的作用。在我国由于早些年健康意识不足，对牙齿的保护工作做的非常不好，统计显示我国的龋齿、牙周炎以及各类牙缺失的问题严重。如在60岁以上的人群中，牙齿的患病率为79.42%；在70岁以上人群中，牙齿患病率达到 100%。中青年人群中患牙病的也不在少数。并且，有研究表明牙齿畸形不仅影响口腔功能和外观，还对个体社会和心理适应有所影响，越来越多的人注重牙齿的健康与美观。
金属基牙科烤瓷修复体的成功与耐用很大程度上取决于合金与烤瓷层的良好结合。合金与烤瓷间的匹配，受到三方面的影响：一是合金与烤瓷的热膨胀系数，二是烤瓷烧结温度与合金熔点的关系，三是金瓷结合界面的润湿状态。合金与烤瓷热膨胀系数的匹配在三个影响因素中占主要地位。当金属和陶瓷两者的热膨胀系数接近或相同时，界面稳定，结合良好，但实际上这种状态往往难以达到。由于陶瓷一般对张应力更敏感，抗压强度远远高于抗张强度，所以一般希望瓷层承受一定的压应力，处于压应力的瓷层还可以抵消部分由热应力或机械应力而加于制品上的张应力，从而提高制品的机械强度和热稳定性。因此设计时，一般希望烤瓷的热膨胀系数稍稍小于金属的热膨胀系数。金－瓷膨胀系数的差异在0－0.5×10-6/℃的范围内就最为理想。但是现有的金属基烤瓷修复体经常发生崩瓷、金瓷结合强度不够等问题，所以对其进行有效改良并制备纳米瓷粉材料很有必要。
发明内容
本发明所要解决的技术问题：针对现有牙科用瓷粉材料金属基烤瓷修复体经常发生崩瓷、金瓷结合强度不够的问题，提供了一种高韧性口腔用纳米瓷粉材料的制备方法。
为解决上述技术问题，本发明采用的技术方案是：
（1）按重量份数计，分别称量45～50份去离子水、10～15份质量分数10％氯化锆溶液、10～15份质量分数5％氨水溶液、35～40份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并超声分散，得分散液并离心分离，得下层沉淀；
（2）将下层沉淀干燥得干燥物，升温加热并保温煅烧，静置冷却至室温并研磨过筛，得改性粉末；
（3）按重量份数计，分别称量45～50份去离子水、1～2份氧化镁、3～5份改性粉末、6～8份纳米氧化铝、3～5份聚甲基丙烯酸、55～60份异丙醇、6～8份氧氯化锆和3～5份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用调节pH至8.5，得前驱体浆液；
（4）将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，静置冷却至室温，将前驱体浆液浇注至模具中，升温加热、保温煅烧，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
步骤（3）所述的调节pH采用的是质量分数5％氨水。
步骤（4）所述的沉积处理为控制激光功率为3～5kW，激光束斑直径为10～15mm，激光照射时间为60～90s，熔炼6～8h。
步骤（4）所述的升温加热为按5℃/min升温至750～850℃。
本发明与其他方法相比，有益技术效果是：
（1）本发明技术方案通过在陶瓷制备模具中沉积钼粉并经熔融包覆改性，通过三元金属硅化物Mo2SiZr的高硬度和金属键与原子键共存的原子间键合性质，使其在与其他金属零部件表面接触而发生摩擦磨损时难于发生金属黏着和变形，有效提高纳米瓷粉的耐磨性能和力学性能；
（2）本发明技术方案纳米氧化锆改性复合瓷粉，由于采用与制备单相凝胶相同的方法，即改变溶液p 值以得到两相混合液体的共同沉淀物，所制备的沉淀物材料具有优异的结合性能，有效提高本发明技术方案中氧化锆对材料的增韧改性程度，在一定程度上提高本发明技术方案的结合强度和力学性能。
具体实施方式
按重量份数计，分别称量45～50份去离子水、10～15份质量分数10％氯化锆溶液、10～15份质量分数5％氨水溶液、35～40份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并置于200～300W下超声分散10～15min，得分散液并置于1500～2000r/min下离心分离10～15min，得下层沉淀并置于110～120℃下干燥1～2h，得干燥物并按5℃/min升温至650～800℃，保温煅烧1～2h，静置冷却至室温并研磨过200目筛，得改性粉末；按重量份数计，分别称量45～50份去离子水、1～2份氧化镁、3～5份改性粉末、6～8份纳米氧化铝、3～5份聚甲基丙烯酸、55～60份异丙醇、6～8份氧氯化锆和3～5份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用质量分数5％氨水调节pH至8.5，得前驱体浆液；将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，控制激光功率为3～5kW，激光束斑直径为10～15mm，激光照射时间为60～90s，熔炼6～8h后，静置冷却至室温，将前驱体浆液浇注至模具中，按5℃/min升温至750～850℃下保温煅烧3～5h，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
实例1
按重量份数计，分别称量45份去离子水、10份质量分数10％氯化锆溶液、10份质量分数5％氨水溶液、35份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并置于200W下超声分散10min，得分散液并置于1500r/min下离心分离10min，得下层沉淀并置于110℃下干燥1h，得干燥物并按5℃/min升温至650℃，保温煅烧1h，静置冷却至室温并研磨过200目筛，得改性粉末；按重量份数计，分别称量45份去离子水、1份氧化镁、3份改性粉末、6份纳米氧化铝、3份聚甲基丙烯酸、55份异丙醇、6份氧氯化锆和3份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用质量分数5％氨水调节pH至8.5，得前驱体浆液；将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，控制激光功率为3kW，激光束斑直径为10mm，激光照射时间为60s，熔炼6h后，静置冷却至室温，将前驱体浆液浇注至模具中，按5℃/min升温至750℃下保温煅烧3h，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
实例2
按重量份数计，分别称量47份去离子水、12份质量分数10％氯化锆溶液、12份质量分数5％氨水溶液、37份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并置于250W下超声分散12min，得分散液并置于1750r/min下离心分离12min，得下层沉淀并置于115℃下干燥2h，得干燥物并按5℃/min升温至750℃，保温煅烧2h，静置冷却至室温并研磨过200目筛，得改性粉末；按重量份数计，分别称量47份去离子水、2份氧化镁、4份改性粉末、7份纳米氧化铝、4份聚甲基丙烯酸、57份异丙醇、7份氧氯化锆和4份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用质量分数5％氨水调节pH至8.5，得前驱体浆液；将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，控制激光功率为4kW，激光束斑直径为12mm，激光照射时间为80s，熔炼7h后，静置冷却至室温，将前驱体浆液浇注至模具中，按5℃/min升温至770℃下保温煅烧4h，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
实例3
按重量份数计，分别称量50份去离子水、15份质量分数10％氯化锆溶液、15份质量分数5％氨水溶液、40份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并置于300W下超声分散15min，得分散液并置于2000r/min下离心分离15min，得下层沉淀并置于120℃下干燥2h，得干燥物并按5℃/min升温至800℃，保温煅烧2h，静置冷却至室温并研磨过200目筛，得改性粉末；按重量份数计，分别称量50份去离子水、2份氧化镁、5份改性粉末、8份纳米氧化铝、5份聚甲基丙烯酸、60份异丙醇、8份氧氯化锆和5份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用质量分数5％氨水调节pH至8.5，得前驱体浆液；将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，控制激光功率为5kW，激光束斑直径为15mm，激光照射时间为90s，熔炼8h后，静置冷却至室温，将前驱体浆液浇注至模具中，按5℃/min升温至850℃下保温煅烧5h，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
将本发明制备的实例1，2，3进行性能测试，具体测试结果如下表表1所示：
表1性能测试表
由上表可知，本发明制备的牙科用瓷粉具有优异的力学性能和导热性能。
Claims (4)
1.一种高韧性口腔用纳米瓷粉材料的制备方法，其特征在于具体制备步骤为：
（1）按重量份数计，分别称量45～50份去离子水、10～15份质量分数10％氯化锆溶液、10～15份质量分数5％氨水溶液、35～40份质量分数1％十二烷基硫酸钠置于三角烧瓶中，搅拌混合并超声分散，得分散液并离心分离，得下层沉淀；
（2）将下层沉淀干燥得干燥物，升温加热并保温煅烧，静置冷却至室温并研磨过筛，得改性粉末；
（3）按重量份数计，分别称量45～50份去离子水、1～2份氧化镁、3～5份改性粉末、6～8份纳米氧化铝、3～5份聚甲基丙烯酸、55～60份异丙醇、6～8份氧氯化锆和3～5份质量分数1％硝酸钇溶液置于三角烧瓶中，搅拌混合并用调节pH至8.5，得前驱体浆液；
（4）将200目钼粉添加至激光熔炼炉中并对石墨模具内壁进行沉积处理，静置冷却至室温，将前驱体浆液浇注至模具中，升温加热、保温煅烧，静置冷却至室温，研磨粉碎并过200目筛，得高韧性口腔用纳米瓷粉材料。
2.根据权利要求1所述的一种高韧性口腔用纳米瓷粉材料的制备方法，其特征在于：步骤（3）所述的调节pH采用的是质量分数5％氨水。
3.根据权利要求1所述的一种高韧性口腔用纳米瓷粉材料的制备方法，其特征在于：步骤（4）所述的沉积处理为控制激光功率为3～5kW，激光束斑直径为10～15mm，激光照射时间为60～90s，熔炼6～8h。
4.根据权利要求1所述的一种高韧性口腔用纳米瓷粉材料的制备方法，其特征在于：步骤（4）所述的升温加热为按5℃/min升温至750～850℃。
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Effective date of registration: 20200907 Address after: 201318 / F, No.16, Lane 500, Furonghua Road, Zhoupu Town, Pudong New Area, Shanghai Applicant after: Dengteng (Shanghai) medical equipment Co.,Ltd. Address before: 213000 No. 35 straight North Street, bell tower, Jiangsu, Changzhou Applicant before: Qian Xing |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20201013 |