CN113105247A - 一种氮化硅陶瓷牙齿的制备方法 - Google Patents
一种氮化硅陶瓷牙齿的制备方法 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 69
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 69
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
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Abstract
本发明公开了一种氮化硅陶瓷牙齿的制备方法，原材料分为氮化硅粉体、超纯水、高纯氧化锌、氧化钇、氧化铝、聚乙烯醇、聚乙烯醇缩丁醛、分散剂0～1％和消泡剂0～0.15％，（1）磨粉：先称取所需氮化硅陶瓷粉体适量，将氮化硅陶瓷粉体装入砂磨机中，向砂磨机中注入超纯水，（2）配方：a相93%以上的氮化硅陶瓷粉体，粒径D50—0.8um占总重量的80‑‑‑92%；高纯氧化锌、氧化钇或氧化铝为助溶剂，粒径均为D50—0.5um；本发明一种氮化硅陶瓷牙齿的制备方法具有牙根无金属成分，自我感觉舒适，缩短了患者术后的适应期、硬度和强度高，患者无需顾忌耐磨性、生物相容性好，优于各种金属或其它非金属材料的优点。
Description
技术领域
本发明涉及制作氮化硅陶瓷种植牙牙根技术领域，具体为一种氮化硅陶瓷牙齿的制备方法。
背景技术
人的牙齿成份是羟基磷酸钙，密度0.79g/cm3，修复和镶补牙齿后患者一般要有很长的适应期，而影响适应的最主要因素是：修复和镶补牙齿材料的比重、温度、硬度和颜色等指标与原牙齿的相似性。氮化硅陶瓷比重是3.23g/cm3（羟基磷灰石的比重是3.19g/cm3），是最佳的无机非金属材料生物陶瓷材料：1、无材料感染风险，陶瓷颗粒不会引发过敏或病理反应；2、极佳的生物相容性，对牙龈相亲，温度与人体相适应，无刺激感觉；3、优良的机械性能指标：耐酸碱腐蚀、表面自润性、耐磨性、硬度高，抗老化和抗刮擦；4、氮化硅对于引起牙龈疾病（牙周炎）的细菌具有杀菌作用，是脊柱内填埋物的材料。然而，氮化硅陶瓷颜色的单调和不易调色，外表的不美观，使其只能用作食牙，或者作为种植牙牙根，本发明的食牙和种植牙牙根是氮化硅陶瓷材料制作的，是一种带患者异物感较小的陶瓷骨架。
发明内容 本发明的目的克服现有技术的不足，提供一种氮化硅陶瓷牙齿的制备方法，具有牙根无金属成分，自我感觉舒适，缩短了患者术后的适应期、硬度和强度高，患者无需顾忌耐磨性、生物相容性好，优于各种金属或其它非金属材料的优点，解决了现有技术中的问题。
为实现上述目的，本发明提供如下技术方案：一种氮化硅陶瓷牙齿的制备方法，所述原材料分为氮化硅粉体、超纯水、高纯氧化锌、氧化钇、氧化铝、聚乙烯醇、聚乙烯醇缩丁醛、分散剂0～1％和消泡剂0～0.15％。
所述制备工艺如下：
（1） 磨粉：先称取所需氮化硅陶瓷粉体适量，将氮化硅陶瓷粉体装入砂磨机中，向砂磨机中注入超纯水；
（2）配方：a相93%以上的氮化硅陶瓷粉体，粒径D50—0.8um占总重量的80---92%；高纯氧化锌、氧化钇或氧化铝为助溶剂，粒径均为D50—0.5um，各占1—5%；增塑剂使用聚乙烯醇、聚乙烯醇缩丁醛等，用量1—3%；分散剂0～1％；消泡剂0～0.15％，得到料浆溶液；
（3） 造粒和制作喂料：将料浆溶液倒出高温搅拌机，倒入造粒、喂料机中，通过抽真空、加热将料浆挤出、切断得到喂料；
（4） 注射成型：将喂料装入注射机中，根据各种规格的成型模具，注射成型得到各种规格的氮化硅陶瓷牙根生坯；
（5）烧结：所述烧结工艺制度为：以1°C /min-20°c /min的升温速率从室温升温到400-600°C保温0-100分钟，以1°C /min-15°c /min的升温速率升温到800°C -1200°C，保温0-100分钟，以1°C /min-10°C /min的升温速率升温到1500-1850°C保温1-10小时，然后以1°C /min-20°C /min的降温速率冷却至室温；
（6）后加工：将烧结后的氮化硅陶瓷牙根毛坯依次经过分类检验、喷砂、预处理和真空无菌封装得到氮化硅陶瓷牙根。
优选的，所述步骤（2）转速控制为300-2500r/m，研磨时间为1---6小时。
优选的，所述步骤（5）脱胶温度20℃----835℃，脱胶速率为2℃/分钟。
优选的，所述步骤（5）烧结温度为835℃～ 1860℃，升温速度为3℃/分钟，最高温度时保温2h。
该发明中未涉及部分均与现有技术相同或可采用现有技术加以实现。
与现有技术相比，本发明的有益效果如下：
1：本一种氮化硅陶瓷牙齿的制备方法先将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水后向砂磨机中加入氧化锌粉体等，之后倒入高温搅拌机中，再依次向高温搅拌机中加入PVA、石蜡、硬脂酸、分散剂、流平剂和引发剂等，混合均匀后进行研磨得到料浆溶液。将料浆溶液倒出高温搅拌机，注入造粒、喂料机中，通过抽真空、加热将料浆挤出、切断得到喂料；将喂料装入注射机中，根据各种规格的成型模具，注射成型得到各种规格的氮化硅陶瓷牙根生坯；最后将氮化硅陶瓷牙根生坯依次进行脱胶---烧结、分类检验、喷砂、预处理和真空无菌封装得到氮化硅陶瓷牙根。其制备工艺简单，操作方便，成本低，制备的陶瓷牙齿无放射性。
具体实施方式
下面结合具体实施例来进一步描述本发明，本发明的优点和特点将会随着描述而更为清楚，但实施例仅是范例性的，并不对本发明的范围构成任何限制，本领域技术人员应该理解的是，在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换，但这些修改和替换均落入本发明的保护范围内。
实施例1
一种氮化硅陶瓷牙齿的制备方法，原材料分为氮化硅粉体、超纯水、高纯氧化锌、氧化钇、氧化铝、聚乙烯醇、聚乙烯醇缩丁醛、分散剂0～1％和消泡剂0～0.15％；
制备工艺如下：
（1）磨粉：先称取所需氮化硅粉体适量，将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水；
（2）配方：选取适量的氧化锌等粉体，加入到砂磨机研磨罐中，在加入适量的超纯水，研磨均匀后倒出，在加入到高温搅拌机中；依次向高温搅拌机中加入PVA、石蜡、硬脂酸、分散剂、流平剂和引发剂等，混合均匀后进行研磨得到料浆溶液，转速控制为300-2500r/m，研磨时间为1--6小时；
（3）造粒和制作喂料：将料浆溶液倒出高温搅拌机，倒入造粒、喂料机中，通过抽真空、加热将料浆挤出、切断得到喂料；
（4）注射成型：将喂料装入注射机中，根据各种规格的成型模具，注射成型得到各种规格的氮化硅陶瓷牙根生坯；
（5）烧结：烧结工艺制度为：以1°C /min-20°c /min的升温速率从室温升温到400-600°C保温0-100分钟，以1°C /min-15°c /min的升温速率升温到800°C -1200°C，保温0-100分钟，以1°C /min-10°C /min的升温速率升温到1500-1850°C保温1-10小时，然后以1°C/min-20°C /min的降温速率冷却至室温；
（6） 后加工：将烧结后的氮化硅陶瓷牙根毛坯依次经过分类检验、喷砂、预处理和真空无菌封装得到氮化硅陶瓷种植牙牙根。
根据以上步骤，先将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水后向砂磨机中添加氧化钇、氧化锌等粉体，之后导入高温搅拌机，并依次向高温搅拌机中加入PVA、硬脂酸、石蜡、交联剂、分散剂和引发剂等，混合均匀后进行研磨得到料浆溶液，将研磨后的料浆注入造粒、喂料机中制得喂料，填入注射成型机后直接得到氮化硅陶瓷牙根生坯；最后将氮化硅陶瓷牙根生坯依次进行脱胶----烧结等，得到氮化硅陶瓷牙根毛坯；其制备工艺简单，操作方便，成本低，制作的陶瓷种植牙牙根缩短患者适应时间和兼顾了患者的舒适感。
实施例2
一种氮化硅陶瓷牙齿的制备方法，原材料分为氮化硅粉体、超纯水、高纯氧化锌、氧化钇、氧化铝、聚乙烯醇、聚乙烯醇缩丁醛、分散剂0～1％和消泡剂0～0.15％；
制备工艺如下：
（1） 粉体研磨：先称取所需氮化硅粉体适量，将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水；
（2） 配方：选取适量的氧化锌粉体，加入到球磨罐中，在加入适量的超纯水，研磨均匀后倒出，加入到高温搅拌机中；依次向高温搅拌机中加入PVA、石蜡、硬脂酸、分散剂、流平剂和引发剂等，混合均匀后进行研磨得到料浆溶液，转速控制为300-2500r/m，研磨时间为1---6小时；
（3）造粒和制作喂料：将料浆溶液倒出高温搅拌机机，倒入造粒、喂料机中，通过抽真空、加热将料浆溶液挤出、切断得到喂料；
（4）注射成型：将喂料装入注射机中，根据各种规格的成型模具，注射成型得到各种规格的氮化硅陶瓷牙根生坯；
（5）烧结：将氮化硅陶瓷牙根生坯进行脱胶------烧结，脱胶温度20℃----835℃，脱胶速率为2℃/分钟；烧结温度为835℃～ 1860℃，升温速度为3℃/分钟，最高温度时保温2h；之后自然降温----冷却；
（6）后加工：将烧结后的氮化硅陶瓷牙根毛坯依次经过分类检验、喷砂、预处理和真空无菌封装得到氮化硅陶瓷牙根。
根据以上步骤，先将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水后向砂磨机中添加氧化钇、氧化锌等粉体，之后导入高温搅拌机，并依次向高温搅拌机中加入PVA、硬脂酸、石蜡、交联剂、分散剂和引发剂等，混合均匀后进行研磨得到料浆溶液，将研磨后的料浆注入造粒、喂料机中制得喂料，填入注射成型机后直接得到氮化硅陶瓷牙根生坯；最后将氮化硅陶瓷牙根生坯依次进行脱胶----烧结等，得到氮化硅陶瓷牙根毛坯；其制备工艺简单，操作方便，成本低，制作的陶瓷种植牙牙根缩短患者适应时间和兼顾了患者的舒适感。
综上：本发明一种氮化硅陶瓷牙齿的制备方法，先将氮化硅粉体装入砂磨机中，向砂磨机中注入超纯水后向砂磨机中添加氧化钇、氧化锌等粉体，之后导入高温搅拌机，并依次向高温搅拌机中加入PVA、硬脂酸、石蜡、交联剂、分散剂和引发剂等，混合均匀后进行研磨得到料浆溶液，将研磨后的料浆注入造粒、喂料机中制得喂料，填入注射成型机后直接得到氮化硅陶瓷牙根生坯；最后将氮化硅陶瓷牙根生坯依次进行脱胶----烧结等，得到氮化硅陶瓷牙根毛坯；其制备工艺简单，操作方便，成本低，制作的陶瓷种植牙牙根缩短患者适应时间和兼顾了患者的舒适感。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内，本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (5)
1.一种氮化硅陶瓷牙齿的制备方法，其特征在于：所述原材料分为氮化硅粉体、超纯水、高纯氧化锌、氧化钇、氧化铝、聚乙烯醇、聚乙烯醇缩丁醛、分散剂0～1％和消泡剂0～0.15％。
2.根据权利要求1所述的一种氮化硅陶瓷牙齿的制备方法，其特征在于：所述制备工艺如下：
（1） 磨粉：先称取所需氮化硅陶瓷粉体适量，将氮化硅陶瓷粉体装入砂磨机中，向砂磨机中注入超纯水；
（2）配方：a相93%以上的氮化硅陶瓷粉体，粒径D50—0.8um占总重量的80---92%；高纯氧化锌、氧化钇或氧化铝为助溶剂，粒径均为D50—0.5um，各占1—5%；增塑剂使用聚乙烯醇、聚乙烯醇缩丁醛等，用量1—3%；分散剂0～1％；消泡剂0～0.15％，得到料浆溶液；
（3） 造粒和制作喂料：将料浆溶液倒出高温搅拌机，倒入造粒、喂料机中，通过抽真空、加热将料浆挤出、切断得到喂料；
（4） 注射成型：将喂料装入注射机中，根据各种规格的成型模具，注射成型得到各种规格的氮化硅陶瓷牙根生坯；
（5）烧结：所述烧结工艺制度为：以1°C /min-20°c /min的升温速率从室温升温到400-600°C保温0-100分钟，以1°C /min-15°c /min的升温速率升温到800°C -1200°C，保温0-100分钟，以1°C /min-10°C /min的升温速率升温到1500-1850°C保温1-10小时，然后以1°C/min-20°C /min的降温速率冷却至室温；
（6）后加工：将烧结后的氮化硅陶瓷牙根毛坯依次经过分类检验、喷砂、预处理和真空无菌封装得到氮化硅陶瓷牙根。
3.根据权利要求2所述的一种氮化硅陶瓷牙齿的制备方法，其特征在于：所述步骤（2）转速控制为300-2500r/m，研磨时间为1---6小时。
4.根据权利要求2所述的一种氮化硅陶瓷牙齿的制备方法，其特征在于：所述步骤（5）脱胶温度20℃----835℃，脱胶速率为2℃/分钟。
5.根据权利要求2所述的一种氮化硅陶瓷牙齿的制备方法，其特征在于：所述步骤（5）烧结温度为835℃～ 1860℃，升温速度为3℃/分钟，最高温度时保温2h。
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