CN106083007A - 金属烤瓷牙遮色瓷素瓷粉及其制备方法 - Google Patents

金属烤瓷牙遮色瓷素瓷粉及其制备方法 Download PDF

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CN106083007A
CN106083007A CN201610402322.8A CN201610402322A CN106083007A CN 106083007 A CN106083007 A CN 106083007A CN 201610402322 A CN201610402322 A CN 201610402322A CN 106083007 A CN106083007 A CN 106083007A
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田念华
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Zhongshan Bangte Biological Technology Co Ltd
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Abstract

本发明涉及金属烤瓷牙遮色瓷素瓷粉及其制备方法。一种金属烤瓷牙遮色瓷素瓷粉，按重量份数计，其原料由碳酸钾11‑15份、碳酸钠7‑9份、碳酸钙0.8‑2份、氧化铝8‑15份、二氧化硅30‑35份、硅酸锆8‑13份、碳酸锂0‑0.2份、硫酸钡0.8‑1.5份、氧化钇0‑0.2份、氧化铈1‑3份、硼酐1‑3份、二氧化钛18‑23份、氧化锌0‑0.2份组成。本发明的金属烤瓷牙遮色瓷素瓷粉原料成本低性能好。

Description

金属烤瓷牙遮色瓷素瓷粉及其制备方法
技术领域
本发明属于牙科材料技术领域，具体涉及金属烤瓷牙遮色瓷素瓷粉及其制备方法。
背景技术
金属烤瓷牙因其优良的理化性能、仿真效果、美学效果、与人体友好的生物相容性，已在牙科临床上广泛应用，成为治疗牙齿缺失的最重要方法之一。
金属烤瓷牙制备工艺通常包括下列几个步骤。第一步首先制备金属基底冠，第二步涂覆遮色瓷并烧结，第三步涂覆体瓷进行烧结，最后涂覆透明瓷(釉瓷)并进行烧结，最后经过加工完成成品。
在中国的牙科材料市场，烤瓷粉系列产品仍然依赖进口，生产成本高。
目前所知的遮色瓷粉的制备方法，如CN166390，CN132235A，均存在因不同批次化工原料中微量杂质的不确定性，用同样的工艺进行生产，其产品难以保证质量的稳定性和一致性，主要原因是陶瓷晶相结构在各种变动中的微量元素的影响下，产生的非逻辑现象，即不同批次的晶相的不同一性，势必造成不同批次产品难以保证热膨胀系数的一致性，存在出现不合格产品的风险。
另外，国内外遮色瓷粉的制备方法，均采用一次烧成工艺，同样的材料组分，不同的烧制程度，生产出的产品膨胀系数有差异。
烤瓷牙常用金属的热膨胀系数为14.1-14.6*10-6/℃，在金瓷结合中，为保证陶瓷体承受压应力，遮色瓷粉的热膨胀系数定在13.3-13.8*10—6/℃。保证遮色瓷粉的热膨胀系数的一致性，提高生产效率，一直的本行业生产的难题。
发明内容
本发明的目的在于针对上述技术上的不足，提供一种原料成本低性能好的金属烤瓷牙遮色瓷素瓷粉。
为解决上述问题，本发明采用如下的技术方案：
一种金属烤瓷牙遮色瓷素瓷粉，按重量份数计，其原料由碳酸钾11-15份、碳酸钠7-9份、碳酸钙0.8-2份、氧化铝8-15份、二氧化硅30-35份、硅酸锆8-13份、碳酸锂0-0.2份、硫酸钡0.8-1.5份、氧化钇0-0.2份、氧化铈1-3份、硼酐1-3份、二氧化钛18-23份、氧化锌0-0.2份组成。
优选地，所述碳酸钾13份、碳酸钠8.4份、碳酸钙1.1份、氧化铝11份、二氧化硅31份、硅酸锆10份、碳酸锂0.1份、硫酸钡1份、氧化钇0.1份、氧化铈2.2份、硼酐1份、二氧化钛21份、氧化锌0.1份。
本发明还提供一种金属烤瓷牙遮色瓷素瓷粉的制备方法。
一种如上所述的金属烤瓷牙遮色瓷素瓷粉的制备方法，其特征在于包括如下步骤:
1)将原料用球磨机混合均匀；
2)将混合均匀的粉料高温锻烧；
3)将高温锻烧后的物料粉碎至D50＝2.5μm；
4)将粉碎后的物料进行高温热处理，然后炉冷；
5)用球磨机分散至D50＝5μm即得所需素瓷粉。
作为进一步改进，高温锻烧时将粉料分为二组分别进行高温锻烧，第一组粉料在830℃保温2小时，然后以105℃/小时均匀升温，至1260℃保温2.3小时，冷却；第二组粉料在830℃保温2.5小时，然后以105℃/小时均匀升温，至1260℃保温5小时，冷却。
作为进一步改进，粉碎后高温热处理前将第一组粉料和第二组粉料按比例混合至需要的热膨胀系数。
作为进一步改进，所述高温热处理是在780℃保温2小时。
与现有技术相比，本发明的优点在于：
1、本发明原料易得，成本低，原料采用硅酸锆，硅酸锆具有优异的化学稳定性，用于制造烤瓷牙遮色瓷粉，在大幅度降低成本的同时提高了产品的性能，硅酸锆价格为8元/kg，而本领域技术人员常用的氧化锆价格为90元/kg。
2、因为烤瓷牙均采用快烧工艺，保温烧结时间仅用一分半钟，对粉体制备工艺要求非常高，既需要控制膨胀系数，同时还要控制晶体形状和晶体数量，采用本发明的高温锻烧工艺，使两组粉体的膨胀系数均控制在12.9-14.0*10—6/℃，且很好地控制晶体形状和晶体数量。
3、本发明方法简单，采用二组粉体分组高温锻烧然后二组粉体再按比例混合，使得粉体膨胀系数可控，产品合格率100％，生产效率更高。
4、本发明素瓷粉制作产品经测试，密度更高，遮色效果更好，抗弯强度更高，化学溶解性更好。
具体实施方式
实施例1
金属烤瓷牙遮色瓷素瓷粉的制备方法如下：
1)按表1进行备料，原料由碳酸钾、碳酸钠、碳酸钙、氧化铝、二氧化硅、硅酸锆、碳酸锂、硫酸钡、氧化钇、氧化铈、硼酐、二氧化钛、氧化锌组成；
2)将原料用球磨机混合均匀，将粉料分为两组；
3)高温锻烧；第一组粉料在830℃保温2小时培养晶核，然后以105℃/小时均匀升温，至1260℃保温2.3小时使晶体长大，然后冷却；第二组粉料在830℃保温2.5小时培养晶核，然后以105℃/小时均匀升温，至1260℃保温5小时使晶体长大，冷却；
4)将两组粉料分别粉碎至D50＝2.5μm；
5)检测两组粉料的热膨胀系数(检测方法及标准见表2，检测结果见表3)，根据混合后粉料所需的热膨胀系数，按照热膨胀系数线性叠加的原理，计算两组粉料的混合比例(计算方法如下，计算结果见表3)，然后按比例将两组粉料混合；
两组粉料混合比例的计算方法：设产品需要的热膨胀系数为C，已检测第一组粉料的热膨胀系数为A,第二组粉料的热膨胀系数为B,设第一组粉料的百分比为X，则第二组粉料的百分比(1-X),根据C＝A*X+B*(1-X)计算得出两组粉料的百分比。
以本实施例为例计算两组粉料的混合比例：第一组粉料的热膨胀系数为
14.0，第二组粉料的热膨胀系数为13.2，需要产品热膨胀系数为13.55，根据13.55＝14.0*X+13.2*(1-X)，计算得出需要第一组粉料的百分比约为44％，第二组粉料的百分比约为56％。
生产中，不限于同一实施例的两组粉料进行混合，也可把不同实施例的两组粉料进行混合。
6)高温热处理，即在780℃保温2小时，然后炉冷，作用是匀化晶体，消除应力；
7)球磨机分散至D50＝5μm即得所需的素瓷粉；
使用时根据需要将素瓷粉配色。
将得到的素瓷粉制作样品进行检测，检测标准及方法见表2，性能见表3。
实施例2
本实施例的原料组成见表1，制备方法同实施例1，检测标准及方法见表2，产品性能见表3。
实施例3
本实施例的原料组成见表1，制备方法同实施例1，检测标准及方法见表2，产品性能见表3。
表1 单位：kg
实施例1 实施例2 实施例3
碳酸钾 0.14 0.13 0.12
碳酸钠 0.084 0.084 0.084
碳酸钙 0.011 0.011 0.011
氧化铝 0.13 0.11 0.09
二氧化硅 0.33 0.31 0.31
硅酸锆 0.10 0.10 0.09
碳酸锂 0.001 0.001 0.001
硫酸钡 0.01 0.01 0.01
氧化钇 0.001 0.001 0.001
氧化铈 0.022 0.022 0.022
硼酐 0.01 0.01 0.02
二氧化钛 0.21 0.21 0.20
氧化锌 0.001 0.001 0.001
表2
表3
从表3可以看出，实施例2硬度、抗弯强度、密度、化学溶解性综合性能最好。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (6)

1.一种金属烤瓷牙遮色瓷素瓷粉，其特征在于：按重量份数计，其原料由碳酸钾11-15份、碳酸钠7-9份、碳酸钙0.8-2份、氧化铝8-15份、二氧化硅30-35份、硅酸锆8-13份、碳酸锂0-0.2份、硫酸钡0.8-1.5份、氧化钇0-0.2份、氧化铈1-3份、硼酐1-3份、二氧化钛18-23份、氧化锌0-0.2份组成。
2.如权利要求1所述的金属烤瓷牙遮色瓷素瓷粉，其特征在于：按重量份数计，所述碳酸钾13份、碳酸钠8.4份、碳酸钙1.1份、氧化铝11份、二氧化硅31份、硅酸锆10份、碳酸锂0.1份、硫酸钡1份、氧化钇0.1份、氧化铈2.2份、硼酐1份、二氧化钛21份、氧化锌0.1份。
3.一种如权利要求1或2所述的金属烤瓷牙遮色瓷素瓷粉的制备方法，其特征在于包括如下步骤:
1)将原料用球磨机混合均匀；
2)将混合均匀的粉料高温锻烧；
3)将高温锻烧后的物料粉碎至D50＝2.5μm；
4)将粉碎后的物料进行高温热处理,然后炉冷；
5)用球磨机分散至D50＝5μm即得所需素瓷粉。
4.根据权利要求3所述的金属烤瓷牙遮色瓷素瓷粉的制备方法，其特征在于：所述高温锻烧时将粉料分为二组分别进行高温锻烧，第一组粉料在830℃保温2小时，然后以105℃/小时均匀升温，至1260℃保温2.3小时，冷却；第二组粉料在830℃保温2.5小时，然后以105℃/小时均匀升温，至1260℃保温5小时，冷却。
5.根据权利要求4所述的金属烤瓷牙遮色瓷素瓷粉的制备方法，其特征在于：粉碎后高温热处理前将第一组粉料和第二组粉料按比例混合至需要的热膨胀系数。
6.根据权利要求3至5任一所述的金属烤瓷牙遮色瓷素瓷粉的制备方法，其特征在于：所述高温热处理是在780℃保温2小时。
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