CN103395982B - 含有钇稳定二氧化锆的牙齿修复体用陶瓷贴面 - Google Patents

含有钇稳定二氧化锆的牙齿修复体用陶瓷贴面 Download PDF

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CN103395982B
CN103395982B CN201310056556.8A CN201310056556A CN103395982B CN 103395982 B CN103395982 B CN 103395982B CN 201310056556 A CN201310056556 A CN 201310056556A CN 103395982 B CN103395982 B CN 103395982B
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玛蒂娜·约翰内斯
罗兰·额赫特
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Hermsdorfer Institut fuer Technische Keramik eV HITK
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Abstract

本发明涉及用于含有钇稳定二氧化锆的牙齿修复体的陶瓷贴面。本发明的目的是使制备具有高挠曲强度和能够极好地附着于钇稳定二氧化锆陶瓷支架的半透明的陶瓷贴面成为可能。根据本发明，为达到此目的，用于由钇稳定二氧化锆构成的牙齿修复体的陶瓷贴面由以下重量百分比的组分制备：a)SiO2：58.0–74.0；b)Al2O3：4.0–19.0；c)Li2O：5.0–17.0；d)Na2O：4.0–12.0；e)ZrO2∶0.5–6.0。

Description

含有钇稳定二氧化锆的牙齿修复体用陶瓷贴面
本申请要求申请日为2007年3月6日的德国专利申请DE10 2007 011 337.6的优先权；本申请是申请日为2008年3月6日、发明名称为“含有钇稳定二氧化锆的牙齿修复体用陶瓷贴面”的中国专利申请No.200880007416.9(原申请，即第一次提出的申请)的分案申请。
技术领域
本发明涉及牙齿修复体用陶瓷贴面，其中陶瓷支架由钇稳定二氧化锆构成。
背景技术
钇稳定二氧化锆是在牙科修复术中用以提高用于牙冠、嵌体和牙桥的陶瓷支架强度的具有极高强度的高性能材料。为了根据天然牙齿的多样性进行精确调整，需要采用陶瓷贴面。目前，陶瓷贴面在修复牙齿抵御压力的能力中显示出弱点。
陶瓷贴面应易于塑形，颜色和邻牙一致，能高度抵御化学制剂，并即使经过直接的热处理也能保持高的挠曲强度，而且其特点是能与陶瓷支架极好地附着。
粉末和浆料通常用作生产陶瓷贴面的起始材料。陶瓷贴面的性质取决于起始材料的化学和晶体学特征以及颗粒大小。
根据美国专利4,798,536A，含有白榴石的牙瓷料是通过玻璃熔融法制备的。白榴石的含量为按重量计35％-60％。具有高膨胀系数13×10-6/K-15×10-6/K的含有白榴石的牙瓷料用于金属冠的贴面。含白榴石晶体的陶瓷贴面的挠曲强度为80MPa。
美国专利4,189,325A提出使用二硅酸锂修复假牙。该参考文献主要关注Li2O-CaO-Al2O3-SiO2材料系统。加入成核剂Nb2O5和Pt以促进结晶。
美国专利4,515,634A提出向Li2O-CaO-Al2O3-SiO2基础系统中加入成核剂P2O5以促进成核和结晶。
已公开的申请DE 197 50 794 A1描述了在热压成型方法中使用二硅酸锂玻璃陶瓷。然而，使用该方法导致了所修复牙齿的边缘强度较低；而且在加工过程中增加了刀具磨损。
DE 103 36 913 A1提出对要修复的牙齿进行二阶段制备。第一步，硅酸锂结晶并机械加工形成牙科制品；通过第二步热处理，硅酸锂转化为更坚硬的二硅酸锂。因此，所修复的牙齿完全由二硅酸锂晶体的玻璃陶瓷构成。
德国专利DE 196 47 739 C2描述了一种能烧结的二硅酸锂玻璃陶瓷和玻璃。烧结起始材料以形成坯料，这些坯料在700℃℃-1200℃的条件下压制以形成牙科制品。所述二硅酸锂玻璃陶瓷在塑性变形中对邻近的铸造包埋材料(casting investment)仅表现出轻微的反应。
EP 1 235 532 A1描述了基于钇稳定二氧化锆生产高强度陶瓷口腔假体的方法。通过该方法生成的陶瓷支架具有大于1200MPa的四点挠曲强度。
发明内容
本发明的目的是使制备具有高挠曲强度和能够极好地附着于钇稳定二氧化锆陶瓷支架的半透明的陶瓷贴面成为可能。
根据本发明，为实现该目的，用于由钇稳定二氧化锆构成的牙齿修复体的陶瓷贴面由以下重量百分比的组分制备：
除了成核剂ZrO2，在以重量计0.2％-8.0％的限度内加入另一种成核剂，例如TiO2，是有利的。
通过在800℃-940℃的范围内设定的温度程序并以可控方式结晶，粉末状起始玻璃加入或不加入单独的晶体添加剂用于陶瓷贴面，并将该陶瓷贴面烧结至钇稳定二氧化锆牙科制品上。
令人惊讶地，通过特定的玻璃陶瓷和设定的温度程序，可获得结合至钇稳定二氧化锆牙科制品上的极高附着强度，该陶瓷贴面为半透明并能够很好地抵御化学制剂。该玻璃陶瓷的主要结晶相包括二硅酸锂。
除了玻璃陶瓷的粉末状的起始玻璃之外，该陶瓷贴面还包括粉末状的晶体作为起始物。经过设定的热处理，粉末状的陶瓷贴面经历了成核，烧结，与钇稳定二氧化锆熔融，以及伴随着微晶体的形成的结晶的过程。
此外，优选将粉末状的二硅酸锂加入到起始玻璃中。二硅酸锂可通过固态反应制备。
TiO2的加入促进了二硅酸锂的成核和结晶过程。因此有利的是，陶瓷贴面由含有以下组分重量百分比的混合物制备：
二氧化锆或二氧化锆的混合物，以及二氧化钛可用作成核剂用于基于硅酸锂材料的陶瓷贴面的控制结晶。二氧化钛的加入促进了硅酸锂向二硅酸锂的转变。
在优选的陶瓷贴面中，除了二硅酸锂之外，也对硅酸氧化钛锂Li2TiOSiO4，硅酸铝锂(β锂辉石)和少量硅酸锂进行结晶。
陶瓷贴面还可以以其晶体部分低于40％形成。在这种情况中，少量使用陶瓷贴面，仅用于颜色匹配和形成牙科陶瓷支架的特别的美学光泽。陶瓷贴面的强度可通过主动压应力(deliberate compressive stresses.)而进一步增强。
元素Ce,Fe,Mn,Sn,V,Cr,In以及稀土族Pr,Nd,Sm,Eu,Tb,Dy和Er的氧化物可用作着色或荧光添加物。
为改进该技术，添加剂La2O3,B2O3,P2O5,CaO,MgO,ZnO和氟化物可按重量计最多4.0％的量各自独立地分别加入。
为生产陶瓷贴面，在温度500℃-680℃进行形核，在800℃-940℃进行熔融和结晶。形核和结晶过程可被中断，将陶瓷贴面在形核过程和结晶过程之间降至室温，保存，然后再加热至结晶温度。
钇稳定二氧化锆和陶瓷贴面之间的附着强度由挠曲测试来测定。为此目的，将粉末状的陶瓷贴面施用于二氧化锆的两个环形棒的末端表面并进行设定的热处理。附着强度由三点挠曲试验测定。
优选与二氧化锆附着力至少为150MPa的陶瓷贴面。
参照具体实施例，以下将更全面的描述本发明。
附图说明
图1氧化锂和二氧化硅固态反应(于940℃反应4小时)后的x-射线衍射图(XRD)；
图2制备陶瓷贴面的典型温度曲线；以及
图3根据本发明的陶瓷贴面的XRD。
具体实施方式
表1显示了用作根据本发明陶瓷贴面的具体实施例的12种混合物。
表1
实例 1 2 3 4 5 6 7 8 9 10 11 12
SiO2 71.0 71.1 62.0 70.5 69.7 61.2 70.5 70.5 69.6 69.6 58.9 60.5
Al2O3 9.0 4.9 17.9 8.9 4.8 17.7 4.9 8.9 8.8 8.8 17.0 17.5
Li2O 12.6 14.9 5.3 12.5 14.6 5.2 14.8 12.5 12.4 12.4 5.0 5.2
Na2O 5.4 3.0 10.9 5.4 2.9 10.8 3.0 5.4 5.3 5.3 10.4 10.5
TiO2 5.0 4.9 1.2 5.0 5.0 2.5
ZrO2 2.0 1.1 3.9 2.0 1.1 3.9 1.1 2.0 2.0 2.0 3.7 3.8
CaF2 0.7 0.7
CaO 0.6
MgF2 0.7
BaF2 1.9
BaO 1.1
P2O5 1.4 0.8
总计 100 100 100 100 100 100 100 100 100 100 100 100
起始玻璃在铂或铂-铑坩埚中于1530℃的温度下熔融，并置于水中淬火制备烧结体(图2)。
为促进可控结晶，淬火的起始玻璃在约580℃±100℃的条件下回火4小时，冷却后粉碎成粉末状。颗粒的大小采用0.6μm-20μm。
粉末状的二硅酸锂可加入到起始玻璃中。该二硅酸锂可通过固态反应制备。
图1表示通过固态反应生成的二硅酸锂的x-射线衍射图(XRD)。
将湿的起始材料施用到钇稳定二氧化锆的牙科陶瓷支架作为陶瓷贴面，于890℃±50℃的条件下熔融并以可控方式结晶。
图2为在陶瓷贴面制备过程中典型的温度曲线。
表1所列的陶瓷贴面的所有12个实例都为半透明。
陶瓷贴面的光学效果和力学抵抗力受陶瓷贴面的结构，以及陶瓷贴面和陶瓷支架相互作用的影响。
陶瓷贴面和钇稳定二氧化锆(TZ3Y)陶瓷支架的膨胀系数(α)必须相互适合。
基于表1的实例，陶瓷贴面和钇稳定二氧化锆的膨胀系数(α)的比较见表2。
表2
实例 1 2 3 6 11 ZrO2
α50-300℃×10-6/K 8.9 8.7 8.9 8.9 8.7 9.6
α50-500℃×10-6/K 9.8 9.8 9.8 9.6 9.3 9.8
钇稳定二氧化锆陶瓷支架与陶瓷贴面之间的附着强度由三点挠曲试验测定。为此目的，陶瓷贴面的粉末施用于两个圆柱形的二氧化锆样品之间并按照图2进行热处理。
表3显示了所选样品的附着强度，其中α为基于三点挠曲试验的附着强度，单位MPa，m为Weibull参数。
表3
实例 1 2 3 12
αMPa 162.1 183.1 173.4 172.4
m 7.6 13.2 3.5 4.4
依赖于组分和热处理，根据本发明的具有高附着强度的陶瓷贴面可能表现出不同的成核和结晶的过程。
参照表1以及温度为890℃±50℃，实例中陶瓷贴面1,4,8,9和10结晶为硅酸锂和二氧化锆的结晶相。二氧化锆作为成核剂。硅酸锂的结晶发生于两个时相阶段。首先，形成硅酸锂Li2SiO3，并通过随后与周围硅酸盐相发生反应，硅酸锂转化为二硅酸锂Li2Si2O5。
参照表1以及温度为890℃±50℃，实例中陶瓷贴面2，5和7生成二硅酸锂、β锂辉石、硅酸氧化钛锂Li2(TiO)(SiO4)和硅酸锂的结晶相。通过加入二氧化钛可加速二硅酸锂Li2Si2O5的结晶。图3为XRD衍射图。

Claims (10)

1.用于陶瓷贴面的起始产品，其含有粉末状起始玻璃和任选地添加的粉末状晶体，其特征在于，所述起始产品包括以下组分：
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
2.根据权利要求1所述的起始产品，其特征在于，除了包括ZrO2外，其还包括0.2–8.0wt％的TiO2。
3.用于形成陶瓷贴面的起始混合物，其特征在于，其包括以下组分：
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
4.根据权利要求1或2所述的起始产品，其特征在于，其各自独立地包括最多达4.0wt％的以下添加剂：La2O3、B2O3、P2O5、CaO、MgO、ZnO和氟化物。
5.根据权利要求4所述的起始产品，其特征在于，其包括以下添加组分：
6.根据权利要求4所述的起始产品，其特征在于，其包括元素Ce、Fe、Mn、Sn、V、Cr、In以及稀土族Pr、Nd、Sm、Eu、Tb、Dy和Er的着色或荧光添加剂氧化物或它们的组合。
7.用于陶瓷贴面的起始产品，其含有粉末状起始玻璃，其特征在于，所述起始产品包括以下组分：
71.1wt％的SiO2；
4.9wt％的Al2O3；
14.9wt％的Li2O；
3.0wt％的Na2O；
5.0wt％的TiO2；和
1.1wt％的ZrO2,
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
8.用于陶瓷贴面的起始产品，其含有粉末状起始玻璃，其特征在于，所述起始产品包括以下组分：
69.7wt％的SiO2；
4.8wt％的Al2O3；
14.6wt％的Li2O；
2.9wt％的Na2O；
4.9wt％的TiO2；
1.1wt％的ZrO2；
0.6wt％的CaO；和
1.4wt％的P2O5,
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
9.用于陶瓷贴面的起始产品，其含有粉末状起始玻璃，其特征在于，所述起始产品包括以下组分：
70.5wt％的SiO2；
4.9wt％的Al2O3；
14.8wt％的Li2O；
3.0wt％的Na2O；
5.0wt％的TiO2；
1.1wt％的ZrO2；和
0.7wt％的CaF2,
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
10.用于对包含钇稳定二氧化锆的牙齿修复体进行贴面的方法，其特征在于，包括以下步骤：
a)将包含粉末状起始玻璃和任选的晶体添加物的起始产品应用至钇稳定二氧化锆牙科制品上；
b)在800℃-940℃的温度范围内将所述包含粉末状起始玻璃和任选的晶体添加物的起始产品烧结至所述牙科制品上，以形成结晶的陶瓷贴面，
其中所述陶瓷贴面包括以下组分：
所述陶瓷贴面包括二硅酸锂作为主要结晶相。
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US20140045674A1 (en) 2014-02-13
US20110030423A1 (en) 2011-02-10
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CN103395982A (zh) 2013-11-20
WO2008106958A3 (de) 2009-11-05
US8987153B2 (en) 2015-03-24
CN101932298A (zh) 2010-12-29
JP2010519986A (ja) 2010-06-10
DE102007011337A1 (de) 2008-09-11
US20150183681A1 (en) 2015-07-02
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