CN1684720A - 陶瓷内修复组件及其制备方法 - Google Patents

陶瓷内修复组件及其制备方法 Download PDF

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Publication number
CN1684720A
CN1684720A CNA038227533A CN03822753A CN1684720A CN 1684720 A CN1684720 A CN 1684720A CN A038227533 A CNA038227533 A CN A038227533A CN 03822753 A CN03822753 A CN 03822753A CN 1684720 A CN1684720 A CN 1684720A
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China
Prior art keywords
oxide
zirconium
rebuilt component
aluminium oxide
interior
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CNA038227533A
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English (en)
Inventor
W·格利恩
T·奥伯巴赫
C·奥尔特曼
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Synthes Bettlach GmbH
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Mathys AG Bettlach
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Publication of CN1684720A publication Critical patent/CN1684720A/zh
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract

由含有氧化铝和(二)氧化锆的陶瓷材料组成的内修复组件，其中(二)氧化锆以未稳定化或稳定化的形式存在。该材料具有氧化铝和(二)氧化锆含量的梯度。与主要含有氧化铝的关节联结区域相比，在拉应力、弯曲应力和扭应力增加的区域内增加(二)氧化锆的含量。该内修复组件的制备可以如此来进行，即用(二)氧化锆淤浆、锆盐溶液、含有锆的溶胶或醇化物或者由两种或更多种前述溶液/流体组成的混合物浸润开孔的、预先烧结的氧化铝基质。制备还可以这样的方式进行，即连续地用氧化铝粉末和(二)氧化锆粉末填充压模，其中在压模的填充期间改变氧化铝和(二)氧化锆的混合比例。

Description

陶瓷内修复组件及其制备方法
本发明涉及由陶瓷材料组成的内修复组件，该陶瓷材料基本上由氧化铝和(二)氧化锆组成，以及涉及该内修复组件的制备方法。
多年来已知氧化铝和(二)氧化锆经证明是合适的陶瓷植入物材料。氧化铝非常坚硬和耐磨。(二)氧化锆是非常具有折断韧性和耐损坏的材料。已知分别由这两种物料之一组成的内修复组件在人工关节中由于出现的摩擦力而不能任意地相互结合在一起。由氧化铝组成的关节配对物的配对经证明是合适的，而氧化铝与氧化锆以及氧化锆与氧化锆的材料配对在文献中是有争议的，因为其在此能够导致非常严重的磨损现象。
EP 1 035 878 B1介绍了对于由陶瓷材料组成的关节配对物的可能的材料配对，其通过具有最佳抗磨损性能的新型结构形态成为可能。该关节配对物由基本上为氧化铝和氧化锆的烧结材料组成，在此关节配对物中的至少一个由添加了0.1-40重量％氧化铝的氧化锆组成。在一个实施例中，将一个由具有高于5重量％的氧化铝含量的氧化锆组成的关节配对物看作是氧化铝组成的关节配对物，且关节的球形关节头的材料比陶瓷关节窝的材料具有更高的氧化锆含量。
从WO 97/31592中获知，在人工髋关节中制备由氧化铝组成的关节窝和由氧化锆组成的关节头。
从US 2002/0031675 A1中获知一种生物医学组件，其由90mol％的二氧化锆组成，其中二氧化锆通过至少2.1mol％的氧化钇而部分地得到稳定，和含有0.05-1重量％的氧化铝。
US 2002/0010070 A1描述了一种生物医学组件，其由用二氧化锆增强的氧化铝组成，其中含有1-69重量％的氧化锆，和二氧化锆通过至少2.1mol％的氧化钇或稀土元素氧化物而得到稳定。
US 6 312 473 B1描述了被由钛或钛合金组成的层所覆盖的植入物组件。该层的开放孔用生物相容性胶合剂浸渍，该胶合剂通过经选择的氧化物而得到增强，包括氧化铝、氧化镁、氧化锆或这些氧化物的组合。
US 4 950 294描述了一种具有由氧化铝、(二)氧化锆和氧化钇组成的基质的植入物组件。该基质的表面不是单晶的，且生物活性层覆盖在该基质表面上。
此外，从EP 1 228 774 A1、EP 0 908 425 A1、JP 09268055 A和JP 11228221 A中获知由氧化铝和(二)氧化锆的复合材料组成的内修复组件。
从WO 02/102275中获知髋关节植入物，在该髋关节植入物中，关节头由金属合金组成，而关节窝由氧化锆组成并视情况含有氧化铝的添加剂。
从DE 44 35 146 C2中获知一种用于产生梯度材料的空隙率梯度的方法，在该方法中，将一个由导电材料组成的多孔体浸入电解池的电解质中，并通过施用电解电流而导致该多孔体材料的阳极电蚀，其中电蚀沿着阳极和阴极之间的连线而变化。
本发明的任务是产生陶瓷的内修复组件，其不仅坚硬和耐磨而且具有折断韧性并耐损坏。
根据本发明，该任务如此得到解决，即该材料具有氧化铝和(二)氧化锆含量的梯度。
该材料具有氧化铝和(二)氧化锆含量的梯度表示，这一陶瓷体系的含量沿着梯度而变化。因此，本发明的内修复组件不具有均匀的物料组成，而是氧化铝和(二)氧化锆的含量在内修复组件之中变化。与此相反，从上述专利文献中获知的由氧化锆和氧化铝组成的材料复合物在物料中的组分分布均匀。
氧化铝的突出的磨损特性应当主要在内修复组件的这些区域中起作用，即在这些区域中陶瓷滑动配对物相互联结而使材料受到摩擦。因此，在这些区域中，氧化铝的含量较高，并可以直至100％。在可预期有应力最大值和表面压力的内修复组件的区域中，应当主要引入(二)氧化锆的特性。因此，在这些区域中，(二)氧化锆的含量较高，并可以直至100％。
向氧化铝中可以加入0-0.3重量％的氧化镁作为烧结助剂，由此防止了晶粒的生长。(二)氧化锆可以未稳定化或稳定化(含有已知用于相稳定的稀土元素氧化物、碱土金属氧化物、氧化钛、氧化铬或氧化铪的添加剂)的形式存在。
由此可以增强陶瓷内修复组件的抗折断性和折断韧性以及耐损坏性。该材料能够消除断裂能。如果在(二)氧化锆颗粒上出现撕裂，那么就会产生撕裂转移，并在(二)氧化锆的立方体的或者四方体的改变(derkubischen bzw.tetragonalen Modifikation)的存在下产生相转变而成为单斜的(二)氧化锆，其中发生能量的消除。四方/立方晶系至单斜晶系的相转变是与体积增加相关的，以致于压挤断裂峰并阻止了裂纹的增长。这一机制是从迄今可使用的增强转变的陶瓷中获知的。
本发明的内修复组件涉及具有物料梯度和粒度梯度的材料，其可以通过两种不同的方法进行制备。
在第一种方法中，在包含稳定剂的经稳定化的(二)氧化锆的情况下，通过(二)氧化锆颗粒(粒度：＜100nm)的浸润，可以向含有0-0.3重量％氧化镁并具有高度开放的孔隙率的预烧结的氧化铝内修复组件(氧化铝基质)中引入(二)氧化锆。内修复组件的预烧结于800-1200℃进行，其中必须避免材料的收缩，由此保持获得用于浸润的孔隙率。材料中梯度的产生借助于类似于淤浆倾注的方法来进行。将含有锆的溶胶(基于胶体或聚合物；H.Richter，Herstellung keramischerNanofiltrationsmembranen aus ZrO2 und TiO2，Dissertation，TUBergakademie Freiberg，Fakultt für Werkstoffwissenschaft undWerkstofftechnologie，1999)、锆盐溶液、锆醇化物或(二)氧化锆淤浆或者由两种或更多种前述溶液/流体组成的混合物(通过例如倾注或喷溅)涂布在可含有至多0.3重量％氧化镁的、预烧结的多孔氧化铝基质上，或者浸润氧化铝基质。含有锆的溶胶、(二)氧化锆淤浆、锆盐溶液、锆醇化物或者由两种或更多种前述溶液/流体组成的混合物可以含有已经提及的稳定剂。依赖于孔体积、孔隙度、流动体系的时间和浓度，使带孔的材料浸润直至一定的深度。固体颗粒沉积在孔的内表面上。在浸润之后干燥内修复组件，这必须温和地操作，因此在物料中不会出现裂纹。在所述干燥之后，紧接着进行排气过程以去除可能存在的有机添加剂。这些可以在溶胶、淤浆、盐溶液或醇化物中含有的有机添加剂必须在随后的烧结之前通过热排气而去除，因为否则在物料中会出现裂纹和缺陷。只要在氧化铝基质中仍然存在充分开放的孔隙率，就可以常常任意地重复浸润、干燥和排气过程。由此可调整氧化铝基质中的各个所希望的(二)氧化锆含量。在随后于1300-1600℃的烧结期间，产生固态的、经分级的和紧密的(无孔的)氧化铝和(二)氧化锆(立方、四方和单斜晶相)的材料复合物。在进行浸润的一侧，可以存在直至100％的(二)氧化锆。(二)氧化锆的浓度从表面至氧化铝基质的内部连续地降低。随后可以通过HIP(热均衡压制)而进一步地压缩。
第一种所述的方法还能够如此应用，即在未稳定化或稳定化(含有已知用于相稳定的稀土元素氧化物、碱土金属氧化物、氧化钛、氧化铬或氧化铪的添加剂)的(二)氧化锆基质中加入添加有0-0.3重量％氧化镁的氧化铝颗粒。该待加入的颗粒以溶胶、淤浆、盐溶液、醇化物或者两种或更多种前述溶液/流体组成的混合物的形式存在。
经浸润的基质还可以是均匀的多孔复合物。因此，基质可以是氧化铝、(二)氧化锆或复合物。该复合物可以由0-100％的氧化铝和与之相应地100-0％的(二)氧化锆组成。(二)氧化锆可以是未稳定化的或者用常规稳定剂(稀土元素氧化物、碱土金属氧化物、氧化钛、氧化铬或氧化铪，这些物质已知用作为相稳定剂)稳定的(二)氧化锆。
在第二种制备方法中，材料中的梯度通过单轴的或者均衡的干压制进行制备。压模连续地用(二)氧化锆粉末和氧化铝粉末填充，其中根据内修复组件的要求或设计连续地改变(二)氧化锆和含有至多0.3重量％氧化镁的氧化铝的混合比例。通过随后的压制制备得到型体。主要组分(二)氧化锆(稳定化的或未稳定化的)和氧化铝的所有混合比例(100％(二)氧化锆和0％氧化铝至100％氧化铝和0％(二)氧化锆)都是可以实现的。陶瓷组件的区域还可以只由氧化铝，只由(二)氧化锆，或者由具有均匀组成的氧化铝和(二)氧化锆构成的复合物组成，其中其他区域由经分级的物料组成。(二)氧化锆还是涉及未稳定化或稳定化的物料。
在成形之后，在两个步骤中进行热处理。在第一步骤中，将仍然在型体中存在的有机物排除，在第二步骤中，将型体于1300-1600℃进行烧结以获得固态的、经分级的和紧密的氧化铝和(二)氧化锆(单斜、四方和立方晶相)的材料复合物。在此，型体还可以通过HIP而进一步地压缩。
还存在这样的可能性，即在可能的预烧结之前或之后实施的排气之后，根据上述的第一种方法将制备得到的型体进行浸润处理。
在两种制备方法中，两个相(氧化铝和(二)氧化锆)各自均匀地相互交融。(二)氧化锆以四方、立方或单斜的改变形式存在。
本发明的陶瓷内修复组件的实施例和材料中产生梯度的原理在附图中进行了描绘，并在下文中进行更详细的描述。附图显示：
图1以截面图显示的由陶瓷组成的髋关节头，
图2以截面图显示的人工关节的陶瓷关节窝，
图3以截面图显示的人工关节的陶瓷嵌体，
图4人工膝关节的陶瓷髁套(Kondylenkufe)，和
图5-7材料中产生梯度的原理。
图1显示了由陶瓷构成的在股骨体上可装配的髋关节头10，该髋关节头用于紧靠着髋关节窝联结，或者将嵌体联结入人工髋关节窝中。关节头10由氧化铝和(二)氧化锆组成，其中材料具有浓度梯度，并且氧化铝和(二)氧化锆的含量沿着梯度而变化。关节头10的表面12受到摩擦，因此具有增加的氧化铝含量。表面12由100％的氧化铝组成。髋关节头10具有一个内锥形梢14，通过其可将髋关节头装配在股骨体上。在关节头10的内锥形梢14中，在将髋关节头10装配在杆圆锥(Schaftkegel)上之后，在切线方向上存在高的表面压力和应力。这就可能出现敲打和碰撞类型的负荷。高的(二)氧化锆含量在此导致比在纯的氧化铝的情况下增加了的抗折断性、折断韧性和耐损坏性。内锥形梢14的表面由将近100％的(二)氧化锆组成。
在材料中具有梯度的关节头10的制备根据上述第一种方法进行：首先制备氧化铝关节头10，并于800-1300℃进行预烧结，从而避免材料的收缩，由此保持获得用于浸润的孔隙率。氧化铝基质含有0.3重量％的氧化镁，并具有高度开放的空隙率。将(二)氧化锆淤浆、含有锆的溶胶、锆盐溶液、锆醇化物或者由两种或更多种前述溶液/流体组成的混合物倾注入内锥形梢区域14中。通过浸润将包含稳定剂的含有锆的物料引入氧化铝基质的多孔区域内。依赖于孔体积、孔隙度、流动体系的时间和浓度，浸润带孔的关节头10直至5mm的所需深度。含有稳定剂的固体颗粒沉积在孔的内表面上。在浸润之后干燥关节头10，这必须小心地施行，因此在物料中不会出现裂纹。在这一干燥之后，紧接着进行排气过程以去除可能存在的有机添加剂。可以多次重复进行浸润、干燥和排气，从而在锥形梢14的内表面上得到将近100％的(二)氧化锆含量。在随后于1300-1600℃的烧结期间，产生固态的、经分级的和紧密的氧化铝和(二)氧化锆(立方、四方和单斜晶相)的材料复合物。随后通过HIP(热均衡压制)而进一步地压缩关节头10。
图2显示了陶瓷关节窝20，和图3显示了陶瓷嵌体30，预先设计将关节头例如图1中所述的髋关节头10紧靠着内侧21、31联结。陶瓷关节窝20和陶瓷嵌体30各具有一个端面和帽状物边缘22、32以及一个底面24、34。在陶瓷关节窝20中，上部区域26具有将近100％的(二)氧化锆含量，以实现在陶瓷头的撞击(在运动期间的杆颈(Schafthals)的碰撞)、半脱位和边缘滑动的情况下的高耐损坏性。在帽形物的顶点27的区域内和在位于陶瓷头和帽形物之间的主关节联结28的区域内，氧化铝含量为100％，以便保证高的耐磨性。对陶瓷嵌体30的上部区域36的要求如同对陶瓷关节窝20的，因此在该区域36中具有将近100％的(二)氧化锆含量。此外，嵌体30的底面34受到拉应力，因为嵌体30通过锥形夹具固定在金属的螺旋式关节窝中。因此，在下部区域39中，(二)氧化锆的含量达到将近100％。(二)氧化锆的含量向着帽形物的顶点37和关节联结区域38连续地降低，因为此处要求特别良好的磨损特性，这通过100％的氧化铝含量来保证。
陶瓷关节窝20和材料中梯度的制备根据上述第二种方法来进行：用氧化铝粉末和(二)氧化锆粉末连续地填充对于制备陶瓷关节窝20所需的压模，其中(二)氧化锆和含有0.3重量％氧化镁的氧化铝的混合比例连续地变化。压模的填充在后来形成关节窝的底面24的区域中开始，并在端面和帽形物边缘22的方向上继续延伸。用氧化铝粉末填充压模，直至达到后来的帽形物的主关节联结区域28的高度。然后在进一步的填充中，在端面和帽形物边缘22的方向上使用氧化铝和(二)氧化锆的粉末混合物，其中(二)氧化锆粉末的含量连续地增加，随后在陶瓷关节窝20的上部区域26中达到将近100％。通过单轴的干压制和随后的加工(Grünbearbeitung)，在添加有机粘合剂的情况下制备陶瓷关节窝20。在成形之后，在两个步骤中进行陶瓷关节窝20的热处理。在第一步骤中，将仍然存在的有机物排出，在第二步骤中，于1300-1600℃进行烧结以获得固态的、经分级的和紧密的氧化铝和(二)氧化锆(单斜、四方、立方晶相)的材料复合物，随后可以通过HIP进行进一步的压缩。
陶瓷嵌体30和材料中梯度的制备根据上述第一种方法来进行：首先，根据与图1中的关节头同样的原理制备由氧化铝构成的经预烧结的嵌体。然后通过用包含已知的稳定剂的(二)氧化锆进行浸润而在材料中产生梯度。为此将嵌体30浸入含有锆的溶胶、氧化锆盐溶液、锆醇化物、氧化锆淤浆或者由前述溶液/流体组成的混合物中，从而覆盖整个外表面，除了用于与关节头联结的内侧区域31之外。预烧结的多孔氧化铝基质可以浸润至大约5mm的深度。在浸润之后，进行干燥和排气。可以任意地常常重复浸润、干燥和排气过程，从而在整个外表面上获得将近100％的(二)氧化锆含量。随后于1300-1600℃进行烧结。可以通过HIP进行进一步的压缩。
图4显示了人工膝关节的陶瓷髁套40，其由氧化铝和(二)氧化锆组成，并且它们的含量沿着梯度变化。通过引入(二)氧化锆来增强整个套40的折断韧性和耐损坏性。承受摩擦和磨损的关节联结面(外侧)42由100％的氧化铝组成，而用于消除刚性以及增强折断韧性和耐损坏性的套内侧44由将近100％的(二)氧化锆构成。
髁套40和材料中梯度的制备根据上述第一种方法来进行：首先，制备由氧化铝构成的髁套40，并于800-1300℃进行烧结。然后在套40的内侧44上涂布(二)氧化锆淤浆、锆醇化物、含有锆的溶胶或锆盐溶液或者由两种或更多种前述溶液/流体组成的混合物，并将预烧结的多孔氧化铝基质从这一侧向外进行浸润。在浸润之后进行干燥和排气。在整个内侧44上得到将近100％的(二)氧化锆含量，其在关节联结面(外侧)42的方向上连续地降低。在外侧42上，髁套40由100％的氧化铝组成。将髁套40于1300-1600℃进行烧结，并可以随后通过HIP进行压缩。
图5-7示意性地显示了，用含有锆的物料浸润氧化铝基质以在材料中形成梯度。预烧结的氧化铝内修复组件50由具有高度开放的孔隙率的氧化铝基质52组成，该氧化铝基质可以含有0-0.3重量％的氧化镁(图5)。通过浸润，在包含稳定剂的经稳定化的(二)氧化锆的情况下，将含有锆的物料60(粒度：＜100nm)引入基质52中(图6)。依赖于孔体积、孔隙度、流动体系的时间和浓度，浸润带孔的材料直至一定的深度。含有锆的颗粒沉积在孔的内表面上，和(二)氧化锆的浓度从表面64至氧化铝基质的内部66连续地降低。在进行浸润的面74上可以存在直至100％的(二)氧化锆，在位于对面的面76上可以存在直至100％的氧化铝(图7)。

Claims (17)

1.由陶瓷材料组成的内修复组件，该陶瓷材料含有氧化铝和(二)氧化锆，其中(二)氧化锆以未稳定化或稳定化(用已知用于相稳定的稀土元素氧化物、碱土金属氧化物、氧化钛、氧化铬或氧化铪的添加剂)的形式存在，其特征在于，该材料具有氧化铝和(二)氧化锆含量的梯度。
2.根据权利要求1的内修复组件，其为人工关节的部件，具有关节联结区域和在使用时承受增加的拉应力、弯曲应力和扭应力的区域，其特征在于，增加的拉应力、弯曲应力和扭应力的区域与关节联结区域相比含有增加含量的(二)氧化锆，而关节联结区域主要含有氧化铝。
3.根据权利要求1或2的内修复组件，其特征在于，存在两个区域，在一个区域中，材料具有将近100％氧化铝和0％(二)氧化锆的混合比，以及在另一个区域中，材料具有0％氧化铝和将近100％(二)氧化锆的混合比。
4.根据权利要求1-3中任一项的内修复组件，其特征在于，在材料中存在氧化铝和(二)氧化锆的浓度梯度。
5.根据权利要求1-4中任一项的内修复组件，其特征在于，在材料中存在与浓度梯度相关联的粒度梯度。
6.根据权利要求1-5中任一项的内修复组件，其特征在于，氧化铝含有含量为0-0.3重量％的氧化镁。
7.制备根据权利要求1-6中任一项的内修复组件的方法，其特征在于，将由开孔的预烧结的氧化铝基质构成的内修复组件用(二)氧化锆淤浆、锆盐溶液、含锆的溶胶或醇化物或者由两种或更多种前述溶液/流体组成的混合物进行浸润，其中将粒径范围为＜100nm的颗粒引入开孔的氧化铝基质中。
8.制备根据权利要求1-6中任一项的内修复组件的方法，其特征在于，将由开孔的预烧结的(二)氧化锆基质(用已知用于相稳定的稀土元素氧化物、碱土金属氧化物、氧化钛、氧化铬或氧化铪的添加剂进行稳定的，或者未稳定化的)组成的内修复组件用含有0-0.3重量％氧化镁的氧化铝颗粒进行浸润，其中将粒径范围为＜100nm的颗粒引入开孔的(二)氧化锆基质中。
9.根据权利要求7或8的方法，其中该内修复组件具有以均匀的、多孔的、由(二)氧化锆和氧化铝组成的复合物的形式存在的基质。
10.根据权利要求7或9的制备内修复组件的方法，其特征在于，浸润例如通过喷溅、浸渍或倾注来进行。
11.根据权利要求7-10中任一项的制备内修复组件的方法，其特征在于，在浸润之后，经浸润的内修复组件的基质经历干燥、排气和烧结过程。
12.根据权利要求7-11中任一项的制备内修复组件的方法，其特征在于，多次重复浸润、干燥和排气过程以增加基质中的(二)氧化锆含量。
13.制备根据权利要求1-6中任一项的内修复组件的方法，其特征在于，压模至少部分连续地用氧化铝粉末和(二)氧化锆粉末的混合物进行填充，其中在压模的填充期间改变氧化铝和(二)氧化锆的混合比例，并且通过压制来制备型体。
14.根据权利要求13的制备陶瓷内修复组件的方法，其特征在于，单轴或均衡地进行压制。
15.根据权利要求13或14的制备内修复组件的方法，其特征在于，将压制出的型体进行排气和烧结。
16.根据权利要求13或14的制备内修复组件的方法，其特征在于，将制备得到的型体进行排气，并随后如权利要求7-11中所述进行浸润处理。
17.根据权利要求7-16中任一项的制备内修复组件的方法，其特征在于，通过热均衡压制来进一步压缩经烧结的型体。
CNA038227533A 2002-09-24 2003-07-28 陶瓷内修复组件及其制备方法 Pending CN1684720A (zh)

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