CN113165876A - 氧化锆材料的制造方法 - Google Patents

氧化锆材料的制造方法 Download PDF

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CN113165876A
CN113165876A CN201980074857.9A CN201980074857A CN113165876A CN 113165876 A CN113165876 A CN 113165876A CN 201980074857 A CN201980074857 A CN 201980074857A CN 113165876 A CN113165876 A CN 113165876A
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zirconia
coating layer
slurry
hydroxyapatite
producing
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武藤光
小林训史
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Obirui Co ltd
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Abstract

本发明实现一种氧化锆材料的制造方法，其能够提供可防止由羟基磷灰石形成的被覆层与氧化锆之间的剥离、作为生物增强材料发挥功能的氧化锆材料。上述氧化锆材料的制造方法中，使羟基磷灰石粉末分散在水中来准备浆料，接着将氧化锆浸渍在浆料中，在氧化锆上形成由羟基磷灰石构成的被覆层，将浆料的羟基磷灰石粉末的浓度设为1％。

Description

氧化锆材料的制造方法
技术领域
本发明涉及氧化锆材料的制造方法。
背景技术
人造骨等所谓植入材料是在天生的骨缺损的情况下与残留的骨接合而能够与骨几乎相同地使用的生物相容性材料。特别是羟基磷灰石在骨头的缺损部的治疗中有用。
并且，氧化锆(二氧化锆：ZrO2)等陶瓷具有化学耐久性、强度特性、耐热性、卫生方面的无害性、生物相容性等各特性，因此作为生物增强材料用于人造骨等。
然而，羟基磷灰石的机械强度低至氧化锆的机械强度的四分之一到十分之一的程度，加工成精密形状的加工性差，因此用途受到限制。
为了消除该样的缺点，研究了在作为基材的氧化锆的表面生成羟基磷灰石作为被覆层的技术方案(例如参照专利文献1)。
专利文献1的目的在于提供一种兼具氧化锆显示的良好机械特性(机械强度和加工性)和羟基磷灰石显示的生物相容性，用于修复骨的缺损部的陶瓷复合材料。特别是其特征在于烧结陶瓷上的被覆层，增大陶瓷与被覆层之间的结合强度。
并且，专利文献1中还公开了利用浆料涂布法和浆料加压浸渍法等在氧化锆上形成被覆层的制造方法。浆料涂布法和浆料加压浸渍法等中的原料的粒度为粒径1μm以下。将该粒径1μm以下的粉末占100％的微细粉末加入水或有机溶剂中，准备固体成分比率为50％～70％的浆料。使用该浆料形成被覆层后，在100℃～500℃的温度范围进行干燥，形成仅有微细粉末的被覆层。
进一步在形成被覆层后烧结被覆层和氧化锆，从而使熔融的被覆层和氧化锆混合，形成混合中间层，生成被覆层与氧化锆彼此之间具有良好的密合性的烧结体。
现有技术文献
专利文献
专利文献1：日本特开昭62－297284号公报。
发明内容
如前所述，为了使氧化锆和羟基磷灰石应用于生物增强材料，需要确保与天生的骨之间的生物相容性和接合部分的机械强度。然而，本申请人验证了专利文献1的陶瓷复合材料，发现微细粉末的固体成分比率为50％～70％的浆料中，导致由羟基磷灰石构成的被覆层从基材剥离，判断不作为生物增强材料发挥功能。
本发明鉴于上述各课题而进行，其目的在于实现一种氧化锆材料的制造方法，其能够提供防止由羟基磷灰石构成的被覆层与氧化锆之间的剥离并作为生物增强材料发挥功能的氧化锆材料。
所述课题通过以下的本发明实现。即本发明的氧化锆材料的制造方法的特征在于，使羟基磷灰石粉末分散在水中来准备浆料，接着将氧化锆浸渍在浆料中，在氧化锆上形成由羟基磷灰石构成的被覆层的氧化锆材料的制造方法中，使浆料的羟基磷灰石粉末的浓度为1％。
并且，本发明的氧化锆材料的制造方法的一个实施方式优选将氧化锆加热到1050℃，接着将氧化锆浸渍在浆料中。
根据本发明的氧化锆材料的制造方法，能够提供一种防止由羟基磷灰石构成的被覆层与氧化锆之间的剥离且作为生物增强材料发挥功能的氧化锆材料。
附图说明
图1是利用本发明的实施例的氧化锆材料的制造方法制造的氧化锆材料的被覆层表面的SEM照片。
图2是对图1中示出的氧化锆材料的被覆层表面在SBF浸渍12小时后进行观察的被覆层表面的SEM照片。
图3是由比较例得到的氧化锆材料的被覆层表面的SEM照片。
具体实施方式
本实施方式的第一特征是在使羟基磷灰石粉末分散在水中而准备浆料，接着将氧化锆浸渍在浆料中，在氧化锆上形成由羟基磷灰石构成的被覆层的氧化锆材料的制造方法中，将浆料的羟基磷灰石粉末的浓度设为1％。
第二特征是进一步将氧化锆加热到1050℃，接着将氧化锆浸渍在浆料中。
根据这些制造方法，能够提供一种防止由羟基磷灰石构成的被覆层与氧化锆之间的剥离、作为生物增强材料发挥功能的氧化锆材料。
应予说明，在本发明中，水为离子交换水。
并且，氧化锆(二氧化锆：ZrO2)是指烧结的没有孔的致密体、或者具有孔径为10μm以上的多个孔的多孔体。
并且，浆料的羟基磷灰石粉末的浓度是指体积百分比浓度。
若将浆料的羟基磷灰石粉末的浓度设定为小于1％，则为了由被覆层生成类骨磷灰石，被覆层在模拟人体体液(Simulated Body Fluid：SBF)中的浸渍时间需要整整7天以上。因此，本申请人通过验证发现具有生物活性的氧化锆材料的量产性下降。
另一方面，如果将浆料的羟基磷灰石粉末的浓度设定为超过1％，则在由羟基磷灰石构成的被覆层与氧化锆之间产生剥离。因此，被覆层与氧化锆间的机械强度不足，不能提供作为生物增强材料发挥功能的氧化锆材料。
另外，为了由被覆层生成类骨磷灰石，被覆层在SBF中的浸渍时间必须为24小时以上。因此，本申请人通过验证发现具有生物活性的氧化锆材料的量产性还是下降。
第三特征是进一步将被覆层的厚度制成0.5μm。
根据该制造方法，除了上述效果，还能够在由羟基磷灰石构成的被覆层上形成类骨磷灰石。
应予说明，本发明中被覆层的厚度是指被覆层的平面方向上的整个面的平均厚度。
本申请人通过验证发现若将被覆层的厚度设定在小于0.5μm和超过0.5μm，则为了由被覆层生成类骨磷灰石，必须将被覆层在SBF中的浸渍时间设定为整整1天以上(24小时以上)。因此，本申请人通过验证发现了具有生物活性的氧化锆材料的量产性下降。
以下，对本发明的实施例进行说明，本发明并不限于以下的实施例。
实施例
以下对本实施例的氧化锆材料的制造方法进行说明。首先，准备成为基材的氧化锆(二氧化锆：ZrO2)和浆料。氧化锆是烧结过的没有孔的致密体或者具有孔径为10μm以上的多个孔的多孔体。考虑应用到生物增强材料，从确保更高的机械强度(特别是弯曲强度)的观点出发，氧化锆更优选含有钇(氧化钇：Y2O3)的氧化锆。具体而言，可举出2Y氧化锆(含有2mol％钇的氧化锆)、2.5Y氧化锆(含有2.5mol％钇的氧化锆)、3Y氧化锆(含有3mol％钇的氧化锆)、8Y氧化锆(含有8mol％钇的氧化锆)。本实施例中，不含有钇，准备在1350℃～1450℃的温度范围内烧结2小时的密度99％的致密体的多晶氧化锆。
另一方面，作为浆料，准备在水中分散有羟基磷灰石粉末的浆料。水为离子交换水。粉末原料的羟基磷灰石(Ca10(PO4)6(OH)2)为市售品的烧结羟基磷灰石，利用球磨机进行粉碎以使平均粒径为0.1μm。使这样的平均粒径0.1μm的羟基磷灰石粉末分散在100重量份水中。分散时，将浆料的羟基磷灰石粉末的浓度以体积百分比浓度计设定为1％。浆料根据需要可以添加分散剂、粘合剂、增粘剂等，本实施例中未使用。
使氧化锆的一部分表面与该浆料接触，将氧化锆浸渍在浆料中。作为浸渍方法，可以向浆料中投入氧化锆、也可以在氧化锆的一部分表面上涂布浆料。本实施例中，在浸渍浆料前，预先将氧化锆加热到1050℃。本申请人通过验证发现通过在浆料中浸渍前，将氧化锆加热到1050℃，从而改善浆料对氧化锆的湿润性、附着性、涂布性。
加热氧化锆后，进行冷却，其后将氧化锆的一部分表面浸渍在浆料中。使浸渍了浆料的氧化锆的表面为研磨面。浸渍时间设定为5分钟。
浸渍后从浆料中除去水，并进行干燥，形成由羟基磷灰石构成、覆盖氧化锆上的被覆层，制成由氧化锆和被覆层构成的氧化锆材料。
将形成的被覆层表面的SEM照片(倍率为1万倍)示于图1。如图1所示，确认了形成的被覆层显示在羟基磷灰石粉末发生粒子结合且在结合的粒子间连通了气孔的多孔结构体的形态。另外，形成的被覆层的厚度为0.5μm。另外，被覆层的厚度是指在被覆层的平面方向遍及被覆层的整面的平均厚度。
形成被覆层后，对被覆层在1050℃～1250℃的温度范围内进行2小时热处理。进一步在该热处理后，在调整为pH7.4、温度36.5℃的模拟人体体液(SBF)中浸渍被覆层，测定生成类骨磷灰石的浸渍时间。使用的SBF具有几乎等于人的血浆的无机离子浓度([mM]：Na+142.0，K+5.0，Mg2+1.5，Ca2+2.5，Cl-148.8，HCO3-4.2，HPO4 2-1.0，SO4 2-0.5)。
结果发现由被覆层生成类骨磷灰石是在至少经过12小时后。浸渍12小时后，如图2(倍率为1万倍)所示，确认了在被覆层的表面生成了类骨磷灰石。
并且，根据本实施例的氧化锆材料的制造方法，如图1所示，确认了能够实现防止由羟基磷灰石构成的被覆层与氧化锆之间的剥离的氧化锆材料。因此，能够提供作为生物增强材料发挥功能的氧化锆材料。
另外，根据本实施例的氧化锆材料的制造方法，除了上述效果，如图2所示，能够在由羟基磷灰石构成的被覆层上形成类骨磷灰石。
另外，确认了通过氧化锆在浆料中浸渍后的热处理，在被覆层与氧化锆之间形成了在氧化锆面内含有钙的改性层(钙锆氧化物)。通过形成这样的改性层提高被覆层与氧化锆相互的密合性。
本申请人通过验证发现如果浆料浸渍后的氧化锆的加热温度小于1050℃，则氧化锆与羟基磷灰石几乎不反应，由羟基磷灰石构成的被覆膜对氧化锆的接合力不会增大。
并且，通过本申请人的验证发现如果氧化锆的加热温度超过1250℃，则不会由被覆层生成类骨磷灰石。
接着，以下对比较例1的氧化锆材料的制造方法进行说明。对于成为基材的氧化锆，准备与上述实施例相同的氧化锆。另一方面，浆料为仅浆料的羟基磷灰石粉末的浓度变更为超过1％的10％。使氧化锆的一部分表面与该浆料接触，将氧化锆浸渍在浆料中。浸渍条件与上述实施例相同。应予说明，比较例1中在浆料浸渍前也预先将氧化锆加热到1050℃。
在浸渍后从浆料中除去水，进行干燥，尝试形成由羟基磷灰石构成、覆盖氧化锆上的被覆层。将制成的结果得到的被覆层表面的SEM照片(倍率为50倍)示于图3。如图3所示，观察到比较例1中被覆层从氧化锆表面剥离。
根据图3的观察结果可知，如果将浆料的羟基磷灰石粉末的浓度设定为超过1％，则由羟基磷灰石构成的被覆层与氧化锆之间发生剥离。比较例1的氧化锆材料中，因为上述剥离的产生，被覆层与氧化锆间的机械强度不足，无法提供作为生物增强材料发挥功能的氧化锆材料。
并且，在测定图3所示的被覆层的未剥离的部位的厚度，结果得到6.0μm～8.0μm的范围的值。在未剥离的被覆层的部位以1050℃进行2小时热处理，热处理后，在pH7.4、温度36.5℃的SBF中浸渍被覆层，测定生成类骨磷灰石的浸渍时间。
其结果可知由被覆层生成类骨磷灰石在至少经过24小时后。因此，发现如果将浆料的羟基磷灰石粉末的浓度设定为超过1％，则为了由被覆层生成类骨磷灰石，被覆层在SBF中的浸渍时间必须为24小时以上，与上述实施例相比，具有生物活性的氧化锆材料的量产性下降。
接着，以下对比较例2所涉及的氧化锆材料的制造方法进行说明。对于成为基材的氧化锆，准备与上述实施例相同的氧化锆。另一方面，浆料为仅浆料的羟基磷灰石粉末的浓度变更为小于1％的0.30％。使氧化锆的一部分表面与该浆料接触，将氧化锆浸渍在浆料中。浸渍条件与上述实施例相同。应予说明，比较例2在浆料浸渍前也预先将氧化锆加热到1050℃。
浸渍后从浆料除去水进行干燥，形成由羟基磷灰石构成、覆盖氧化锆上的被覆层，制成由氧化锆和被覆层构成的氧化锆材料。形成的被覆层的厚度在0.1μm～0.3μm的范围内。
在被覆层以1050℃进行2小时热处理，在热处理后，在pH7.4、温度36.5℃的SBF浸渍被覆层，测定类骨磷灰石所生成的浸渍时间。
其结果可知由被覆层生成类骨磷灰石在至少经过整整7天(168小时)后。因此，发现如果将浆料的羟基磷灰石粉末的浓度设定为小于1％，则为了由被覆层生成类骨磷灰石，则被覆层在SBF中浸渍的时间必须为整整7天以上，与上述实施例相比，具有生物活性的氧化锆材料的量产性下降。
根据以上的实施例、比较例1和比较例2，可知如果将被覆层的厚度设定为小于0.5μm和超过0.5μm，则为了由被覆层生成类骨磷灰石，则被覆层在SBF中的浸渍时间必须设定为整整1天以上(24小时以上)。因此发现与将被覆层的厚度设定为0.5μm的实施方式相比，具有生物活性的氧化锆材料的量产性下降。
另一方面，即使将被覆层的厚度设定为0.5μm，如果被覆层在SBF中的浸渍时间小于12小时，则不会由被覆层生成类骨磷灰石，得不到作为生物增强材料发挥功能的氧化锆材料。

Claims (3)

1.一种氧化锆材料的制造方法，使羟基磷灰石粉末分散在水中来准备浆料，接着，将氧化锆浸渍在浆料中，在氧化锆上形成由羟基磷灰石构成的被覆层的氧化锆材料，其中，将浆料的羟基磷灰石粉末的浓度设为1％。
2.根据权利要求1所述的氧化锆材料的制造方法，其中，将所述氧化锆加热到1050℃，接着将所述氧化锆浸渍在所述浆料中。
3.根据权利要求1或2所述的氧化锆材料的制造方法，其中，将所述被覆层的厚度制成0.5μm。
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