CN103080033A - 针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷以及其涂覆方法 - Google Patents

针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷以及其涂覆方法 Download PDF

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CN103080033A
CN103080033A CN2011800408782A CN201180040878A CN103080033A CN 103080033 A CN103080033 A CN 103080033A CN 2011800408782 A CN2011800408782 A CN 2011800408782A CN 201180040878 A CN201180040878 A CN 201180040878A CN 103080033 A CN103080033 A CN 103080033A
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quality
facing
pottery
glass
zirconium dioxide
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CN103080033B (zh
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马丁纳·约翰内斯
罗兰德·埃尔特
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Abstract

本发明涉及针对牙科修复体的饰面陶瓷，其中，支架陶瓷由钇稳定二氧化锆制成。本发明基于以下任务，即，研发针对由钇稳定二氧化锆制成的牙科修复体的基于二硅酸锂的半透明饰面陶瓷以及用于施布该饰面陶瓷的方法。该饰面陶瓷应该不含有白榴石、偏硅酸锂或β-锂辉石并且具有非常良好的化学稳定性、对二氧化锆的高附着强度以及良好的表面品质。根据本发明，在钇稳定二氧化锆上的饰面陶瓷的情况下通过如下方式来解决该任务，即，该饰面陶瓷由以下组分制成：a）SiO2 55.0-72.5质量%；b）Nb2O5 6.0-19.8质量%；c）B2O3 1.0-9.0质量%；d）Al2O3 1.2-6.0质量%；e）Li2O 5.0-16.5质量%；f）Na2O 1.4-11.0质量%；g）ZrO2 0.5-4.0质量%，并且在饰面陶瓷的表面上设有在结晶期间构造的薄玻璃层。

Description

针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷以及其涂覆方法
技术领域
本发明涉及用于牙科修复体的饰面陶瓷，其中，支架陶瓷由钇稳定二氧化锆制成。
饰面陶瓷的性质通过起始材料的化学组成、晶体相、晶体结构以及粒度来确定。目标在于，满足对饰面陶瓷的高机械的、化学的和美学的要求，并且同时降低在饰面陶瓷的建模中的制备耗费。
背景技术
为了牙科修复体的饰面，通过含白榴石的牙科陶瓷提供了现有技术。在专利US4,798,536A中，白榴石含量处在35至60重量%的范围内。带有白榴石晶体的饰面陶瓷的弯曲断裂强度大约为80MPa。
在专利US4,515,634A中建议，在基础系统Li2O-CaO-Al2O3-SiO2中添加成核剂P2O5用以改善晶核形成和结晶。
在DE 197 25 552A1中描述了用于陶瓷牙科修复体的碱性硅酸盐玻璃。这些牙科材料优选地含有磷灰石晶体。在所描述的磷灰石玻璃陶瓷中应该以限定的摩尔比例1:0.02至1.5:0.03至4.5含有组分CaO:P2O5:F。
在专利文件DE 10 2004 013 455 B3中描述了以磷酸盐和不含氟的硅氧磷灰石为基础的磷灰石玻璃陶瓷以及用于它们的制备的方法和应用。作为晶体相，除了氧磷灰石之外也可出现白榴石。
在专利文件DE 196 47 739 C2中描述了能烧结的二硅酸锂玻璃陶瓷以及玻璃。将起始材料烧结为坯料。这些坯料在700℃至1200℃下被压为牙科产品。在该塑性成形中，所描述的二硅酸锂玻璃陶瓷仅具有与相邻的填料极小的反应。
公开文献DE 197 50 794 A1描述了针对在热压方法中的应用的二硅酸锂玻璃陶瓷的使用。然而已表明的是，在应用该方法的情况下在已修复的牙齿上的边缘强度不足并且在后处理中发生高工具磨损。
DE 103 36 913 A1建议，在两个阶段中完成待修复的牙齿。在第一阶段中，将偏硅酸锂进行结晶，通过机械加工将偏硅酸锂加工成牙科产品。在第二温度处理中，将偏硅酸锂转化为更牢固的二硅酸锂。
在专利文献WO2008/106958A2中描述了具有很高强度和对钇稳定二氧化锆更好附着的饰面陶瓷。在所描述的饰面陶瓷的情况下，除了二硅酸锂之外还出现β-锂辉石、偏硅酸锂的结晶和二氧化硅的不同的相。
基于钇稳定二氧化锆，在EP 1 235 532 A1中描述了用于制备高强度陶瓷牙齿替代物的方法。根据该方法制备的支架陶瓷具有大于1200MPa的4点弯曲断裂强度。
发明内容
本发明的任务在于，研发针对由钇稳定二氧化锆制成的牙科修复体的基于二硅酸锂的半透明饰面陶瓷以及用于施布该饰面陶瓷的方法。该饰面陶瓷应该不含有白榴石、偏硅酸锂或β-锂辉石并且具有非常良好的化学稳定性、对二氧化锆的高附着强度以及良好的表面品质。
根据本发明，在钇稳定二氧化锆上的饰面陶瓷的情况下该任务通过如下方式来解决，即，饰面陶瓷由以下组分制成：
a)SiO2   55.0-72.5质量%
b)Nb2O5  6.0-19.8质量%
c)B2O3   1.0-9.0质量%
d)Al2O3  1.2-6.0质量%
e)Li2O   5.0-16.5质量%
f)Na2O   1.4-11.0质量%
g)ZrO2   0.5-4.0质量%
并且在该饰面陶瓷的表面上设有在结晶期间构造的薄玻璃层。
二硅酸锂形成了饰面陶瓷的主晶体相。符合期望但不是强制必须的是，除了二硅酸锂之外还部分地结晶出铌氧化物。铌氧化物不嵌入或者说仅以很少的量嵌入二硅酸锂的结构中。借助于受控制的结晶，使富铌相紧邻二硅酸锂地积聚。
通过结晶工艺对相组成的改变导致了富铌氧化物的玻璃相。富铌氧化物的玻璃相使得饰面陶瓷的非常高的表面品质成为可能，从而使得不需要另外的烧釉（Glanzbrand）。
为了颜色适配或者说荧光性可以给饰面陶瓷添加染色的元素或者说色素。这些单个的颜色组分的浓度应该最高为3.0质量%。
为了技术改造可以相互不依赖地添加添加物La2O3、BaO、CaO、MgO、ZnO、P2O5、TiO2和氟化物，其中，所列举的添加物的浓度以其总量最大在直至4.0质量%的范围中。
饰面陶瓷具有对二氧化锆的非常良好的附着。因此不透明物（Opaker）或者说内衬物（Liner）的使用不是强制必须的。
可以借助于层技术将饰面陶瓷的所列举的起始材料作为粉末施布到钇稳定二氧化锆上。以限定的研磨工艺也可以将粉末加工成借助于喷射来施布的粉浆（Schlicker）。在随后的结晶之后产生了具有高表面品质的饰面陶瓷。
该饰面陶瓷使得在牙科炉中的温度处理与后续的激光处理的结合成为可能。为此，将饰面陶瓷的涂覆到支架陶瓷上的起始材料借助于牙科炉在850℃至910℃或者说911℃至940℃的温度范围内烧结。受控制的结晶在850℃至910℃温度范围内进行，其中，形成的饰面陶瓷具有高表面品质。如此制成的饰面陶瓷已经可以用于牙科修复体。借助于激光的使用，在进一步的方法步骤中的饰面陶瓷的局部玻璃化是可行的。
同样可行的是，饰面陶瓷的起始材料在911℃至940℃温度范围内烧结到支架陶瓷上并且在进一步的方法步骤中借助于激光来诱发局部的结晶。
饰面陶瓷可以以多个层形式被涂覆。对二氧化锆的非常良好的附着以及非常良好的表面品质使得如下成为可能，即，一个喷射层对于饰面工艺来说已经足够了。
附图说明
以下应结合实施例和附图对本发明进行更详细地阐述。在此：
图1示出了用于饰面陶瓷制备的可行的温度分布；
图2示出了在900℃的温度处理之后的根据本发明的饰面陶瓷的伦琴射线衍射图（XRD）；
图3示出了在二氧化锆上的饰面陶瓷的接合结构；以及
图4示出了用于通过激光诱发结晶制备饰面陶瓷的温度分布。
具体实施方式
在以下表格1中显示了典型的组成。
[表格0001]
表格1
示例 1 2 3 4 5 6 7 8 9
质量% 质量% 质量% 质量% 质量% 质量% 质量% 质量% 质量%
SiO2 62.5 65.6 56.2 65.4 65.5 64.5 61.5 63.8 64.2
Nb2O5 19.0 15.4 18.2 10.8 13.1 12.1 6.7 9.9 12.8
B2O3 1.1 1.4 3.0 2.7 1.4 1.8 6.5 3.0 1.5
Al2O3 1.4 1.5 4.3 2.5 2.0 3.0 4.7 4.0 1.9
Li2O 13.5 13.7 5.2 11.4 12.5 11.4 6.3 9.9 12.2
Na2O 1.5 1.4 9.5 5.3 4.0 4.8 10.5 6.1 3.9
ZrO2 1.0 1.0 3.6 1.9 1.5 1.6 3.8 2.0 1.5
MgO - - - - - 0.8 - 1.3 -
TiO2 - - - - - - - - 2.0
-
总量 100 100 100 100 100 100 100 100 100
钇稳定二氧化锆作为支架陶瓷被用于牙科修复体。该牙科修复体可以有目地地染色。在100℃至500℃温度范围中，钇稳定二氧化锆具有11.1×10-6/K的热膨胀系数α。
对于根据本发明所描述的饰面陶瓷来说，热膨胀系数α100℃至500℃处在9.5×10-6/K和11.0×10-6/K之间的界限中。
在钇稳定二氧化锆与饰面陶瓷之间的附着强度的确定以三点弯曲试验来进行。为此，将粉末状的饰面陶瓷施布到两个由二氧化锆制成的圆棒的端面上并经受限定的温度处理。
根据所描述的方法测得的附着强度应该≥100MPa。
化学稳定性根据DIN EN6872:2009-1ISO来确定并且在根据本发明的饰面陶瓷的情况下<50μg/cm2。
在表格2中登记了相对相应于表格1针对示例4和5的组成的膨胀系数α100℃至500℃、附着强度和化学稳定性的特征值。
[表格0002]
表格2
特征值 示例4 示例5
α100℃至500℃ 10.4×10-6/K 10.1×10-6/K
附着强度 148MPa 130MPa
化学稳定性 20.3μg/cm2 37μg/cm2
为了制备饰面陶瓷在图1中绘制出了工艺上的流程。将在图1中显示的起始玻璃的组成在1400℃温度下在铂坩埚或陶瓷坩埚中熔化并为了制备玻璃烧结料在水中浇铸。
为了支持受控制的结晶，经玻璃烧结的原玻璃在540±50℃下被退火大约4小时并在冷却后被粉末化。投入使用的颗粒大小在0.3μm和30μm之间。
饰面陶瓷的结晶在760℃温度下时就已经开始了。在760℃至840℃的温度范围中，除了二硅酸锂之外出现了偏硅酸锂和方英石(Christobalit)晶体相。伴随温度的提高，偏硅酸锂和方英石晶体相溶解。所述受控制的结晶在850℃至940℃的温度范围内进行。针对900℃的结晶温度，在图2中显示了伦琴射线衍射图（XRD）。
在结晶期间，不仅在表面上还在相对钇稳定二氧化锆的界面上形成了薄玻璃层。在表面层上的该薄玻璃层是针对饰面陶瓷的重要品质标准，并且使得经济的加工技术成为可能。在图3中借助于扫描电子显微镜绘制出了饰面陶瓷的接合结构。
饰面陶瓷的涂覆既可以作为膏状物借助于毛刷进行也可通过喷射进行。对于薄层的经济的涂覆而言优选喷射，其中，既可以单层地进行喷射也可以多层地进行喷射。
另外的方法路径通过如下方式给出，即，将饰面陶瓷在约1000℃的温度下作为透明玻璃熔融到由钇稳定二氧化锆制成的支架陶瓷上。在此，玻璃的熔融既可以通过陶瓷炉进行也可以通过激光的使用进行。
在液相温度以上施布到钇稳定二氧化锆上的饰面陶瓷用作为针对在饰面陶瓷中激光诱发结晶的起始材料。通过激光的限定的使用可行的是，将已施布的层部分地玻璃式地进行设计或在确定的范围内经受有目地的结晶。根据图4进行借助于激光的结晶的可行的流程。

Claims (9)

1.针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷，其特征在于，所述饰面陶瓷含有以下组分：
a)SiO2   55.0-72.5质量%
b)Nb2O5  6.0-19.8质量%
c)B2O3   1.0-9.0质量%
d)Al2O3  1.2-6.0质量%
e)Li2O   5.0-16.5质量%
f)Na2O   1.4-11.0质量%
g)ZrO2   0.5-4.0质量%。
2.针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷，其特征在于，所述饰面陶瓷含有以下组分：
a)SiO2   58.0-68.0质量%
b)Nb2O5  10.0-19.8质量%
c)Al2O3  1.2-6.0质量%
d)Li2O   8.0-16.5质量%
e)Na2O   1.4-8.0质量%
f)ZrO2   0.5-4.0质量%。
3.根据权利要求1或2所述的饰面陶瓷，其特征在于，附加地含有以下组分TiO2、La2O3、MgO、CaO、ZnO、BaO、P2O5和/或氟化物中的至少一种，其中，所有添加的组分的总浓度最大在直至4.0质量%的范围内。
4.根据权利要求1或权利要求2所述的饰面陶瓷，其特征在于，单个地或以组合的形式含有以下元素Fe、Sn、Ce、Mn、V、Cr、Pr、Tb、Nd、Sm、In、Eu、Dy的氧化物或氟化物以及色素，作为染色的或发荧光的添加物。
5.用于对由钇稳定二氧化锆制成的牙科修复体利用根据权利要求1至4中任一项所述的饰面陶瓷进行饰面的方法，其特征在于以下方法步骤：
a）将在1400℃下熔融的玻璃在水中进行玻璃烧结；
b）将经玻璃烧结的玻璃在490℃至590℃的温度下且在两个至六个小时的时长中进行退火以形成晶核；
c）在冷却后将退火的玻璃机械地粉末化至0.3μm和30μm之间的颗粒尺寸；
d）将预处理的粉末转化成膏状物或粉浆并且涂覆到所述牙科修复体上；
e）执行在850℃和910℃之间的范围中的温度处理，并且结晶出二硅酸锂；
f）借助于受控制的结晶使富铌氧化物相紧邻二硅酸锂地积聚，由此在表面上支持薄玻璃层的形成，从而使得不需要特别的烧釉。
6.根据权利要求5所述的方法，其特征在于，在方法步骤f）之后借助于激光来局部地熔融二硅酸锂晶体相，以便提高所述饰面陶瓷的半透明度或者说透明度。
7.用于对由钇稳定二氧化锆制成的牙科修复体利用根据权利要求1至4中任一项所述的饰面陶瓷进行饰面的方法，其特征在于以下方法步骤：
a）将在1400℃下熔融的玻璃在水中进行玻璃烧结；
b）将经玻璃烧结的玻璃在490℃至590℃的温度下且在两个至六个小时的时长中进行退火以形成晶核；
c）在冷却后将退火的玻璃机械地粉末化至0.3μm和30μm之间的颗粒尺寸；
d）将预处理的粉末转化成膏状物或粉浆并且涂覆到所述牙科修复体上；
e）执行在911℃和940℃之间的范围内的温度处理，并且借助于激光来诱发二硅酸锂晶体相。
8.根据权利要求5至7所述的方法，其特征在于，通过加入水和/或有机助剂将预处理的粉末转化为膏状物或粉浆。
9.根据权利要求5至8所述的方法，其特征在于，通过喷射进行粉浆的涂覆。
CN201180040878.2A 2010-08-24 2011-08-18 针对由钇稳定二氧化锆制成的牙科修复体的饰面陶瓷以及其涂覆方法 Active CN103080033B (zh)

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