CN101250638A - 多孔金属泡沫结构及其制造方法 - Google Patents

多孔金属泡沫结构及其制造方法 Download PDF

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CN101250638A
CN101250638A CNA2008100856651A CN200810085665A CN101250638A CN 101250638 A CN101250638 A CN 101250638A CN A2008100856651 A CNA2008100856651 A CN A2008100856651A CN 200810085665 A CN200810085665 A CN 200810085665A CN 101250638 A CN101250638 A CN 101250638A
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liquid
metal
pore
powder
forming material
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H·刘
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DePuy Products Inc
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DePuy Products Inc
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    • Y10T428/12479—Porous [e.g., foamed, spongy, cracked, etc.]

Abstract

本发明描述了多孔金属泡沫结构及其制造方法。优选该方法包括下述步骤：将可液体提取的造孔剂与金属粉末在液体中混合，其中造孔剂可溶于该液体，因此形成混合物，压制该混合物形成坯体以及将造孔剂从坯体中溶去以形成金属骨架。

Description

多孔金属泡沫结构及其制造方法
技术领域
[0001]本发明涉及多孔金属泡沫结构及其制造方法。
背景技术
[0002]多孔金属泡沫结构具有广泛的用途，包括用做医疗上的植入物。这种结构中的多孔结构可以通过将金属粉末与造孔剂(PFA)混合，然后再将混合物压制成所需要的形状从而制成坯体来获得。将PFA除去之后，再将金属骨架烧结从而得到多孔金属泡沫结构所需要的性能。
[0003]一种从坯体中除去PFA的方法是“烧完”PFA。这会引起很多潜在的问题，例如污染炉子，由于在金属和PFA之间发生反应而导致在多孔结构中生成不良金属化合物，并且相比较而言会使用大量能量。某些储存问题，包括有害气体味的形成，也与用这种方法制成的坯体有关。
[0004]因此，需要另外一种方法生产多孔金属泡沫结构。
发明内容
[0005]本发明一方面提供一种方法，包括将可液体提取的造孔剂与金属粉末在液体(Liquid)中混合，其中造孔剂可溶于该液体，因此形成用于压制成坯体的混合物。然后将造孔剂从坯体中溶解形成金属骨架，再将该骨架烧结以形成烧结金属泡沫结构，例如多孔金属植入物。本发明还提供通过该方法制造的多孔金属植入物和其它烧结泡沫结构。
附图说明
[0006]通过参考无标度(non scale)的附图，本领域技术人员可以更好地理解本发明的众多目的和优点，它们通过示例提供，但是不能用来限制本发明。
[0007]图1为根据本发明一实施例制造多孔金属植入物的工艺示意图表。
[0008]图2为烧结金属泡沫结构的图。
[0009]图3为图2中的烧结金属泡沫结构的侧视图。
[0010]图4为图2中的烧结金属泡沫结构的细节图。
[0011]图5为图2中的烧结泡沫金属结构的光学显微图像。
[0012]图6为烧结金属泡沫结构的200倍扫描电子显微(SEM)图像。
[0013]图7为烧结金属泡沫结构的700倍扫描电子显微(SEM)图像。
具体实施方式
[0014]本发明提供一种方法，包括将可液体提取的造孔剂(PFA)与金属粉末在液体中混合，在该液体中PFA是可溶于的。已知的可能的PFA/液体组合包括可溶于有机液体的PFA与有机液体的组合，或者可溶于非有机液体的PFA与非有机液体的组合。
[0015]在某些实施例中，液体是含水的。最好是，液体包含至少约75％重量百分比的水，更好是，至少约90％重量百分比的水，更优选为至少约95％重量百分比的水。典型的液体包括水(例如反渗透水，去离子水，蒸馏水，和/或脱氧水)或含水的碳水化合物溶液。
[0016]尽管所用液体的量由金属粉末和PFA的性能以及所采用的工艺条件决定，但是我们发现所使用的每100cm3预压制的混合物应该使用约450μL到约1050μL的液体，更好的是每100cm3预压制的混合物使用约600μL到约750μL的液体。
[0017]根据本发明的PFAs为可溶于相关液体的颗粒材料。典型的造孔剂包括氯化钠，氯化铵，氯化钙，氯化镁，氯化铝，氯化钾，氯化镍，氯化锌，碳酸氢铵，磷酸氢钠，磷酸二氢钠，磷酸二氢钾，磷酸氢钾，亚磷酸氢钾，磷酸钾，硫酸镁，硫酸钾，碱土金属卤化物，结晶碳水化合物(包括属于单糖，二糖和三糖的蔗糖和乳糖)，聚乙烯醇(PVA)，聚乙烯氧化物，聚丙烯蜡(例如可从Micro Powders公司得到，Tarrytown，纽约，商标为PROPYLTEX)，羧甲基纤维素钠(SCMC)，聚乙二醇-聚丙烯-聚乙二醇共聚物(PEG-PPG-PEG，例如可从BASF公司得到，Ludwigshaften，德国，商标为PLURONIC)，或者其混合物。
[0018]PFA可以具有适于制造孔径尺寸和孔径分布的多种颗粒尺寸和粒度分布。某些优选的颗粒尺寸范围为约200μm到约600μm，约200μm到约350μm，和约350μm到约550μm。
[0019]实际上，粉末冶金领域中已知的各种类型的金属粉末都可以用于本发明的方法。优选的金属粉末为由钛，钴，铬，镍，镁，钽，铌，锆，铝，铜，钼，钨，不锈钢，或其合金(例如，Co-Cr合金)所制成的金属粉末。在一实施例中，金属粉末为钛或钛合金，例如Ti-6Al-4V。
[0020]金属粉末也可以具有多种颗粒尺寸和粒度分布。某些优选的颗粒尺寸范围为约20μm到约100μm，约25μm到约50μm，以及约50μm到约80μm。
[0021]本领域技术人员可以发现：金属粉末和PFA的比例依赖于要生产的结构类型而变化。在本发明的某些实施例中，金属粉末与PFA的比例为约40∶60到约10∶90，优选为与PFA的比例约为25∶75。
[0022]将金属粉末，PFA和液体混合后，所得混合物被压制形成坯体。压制步骤可以采用本领域中多种现有技术中的任何一种，包括单轴模具冲压，双轴模具冲压，或冷等静压或橡胶等静压。在本发明的某些实施例中，压制力为约20ksi到约60ksi，优选为约30ksi到约45ksi。一旦成形，就可以采用本领域中的任一种现有技术对坯料进行机加工，例如切削、铣削、车削、钻孔和/或平面加工。
[0023]可以使用能溶解PFA的任何液体将PFA从坯体中除去，因而现出金属骨架。由于在压制前将液体与金属粉末和PFA混合，所以溶解液最好含水，更优选为水(例如反渗透水，去离子水，蒸馏水，和/或脱氧水)或含水的碳水化合物溶液。用于溶解PFA的液体与压制前将金属粉末和PFA混合的液体可以相同或不同，例如，在各自液体中成分的化学同一性和/或它们的相对比率可以相同或不同。
[0024]溶解步骤可以通过例如将坯体浸入在包含可溶解坯体的液体的容器中来实现，或通过使流动的可溶解坯体的液体与坯体接触来实现。用在溶解步骤中的液体的温度范围为高于其冰点但低于其沸点，优选为约50°F到约176°F(约10℃到约80℃)。可以实施影响溶解的公知的某些步骤，例如，容器中的溶液可以为循环的或者容器中的部分溶液周期性的被新溶液代替。
[0025]除去PFA后得到的金属骨架也可以被机加工，例如切削、铣削、车削、钻孔和/或平面加工该骨架。
[0026]通常通过烧结金属骨架来赋予其所需要的性能。虽然期望可以使用所有合适的烧结条件，但通常在温度为约2100°F到约2700°F(优选为约2500°F)和/或约2小时到约10小时(优选为约3小时到约6小时)的条件下来执行钛或Ti-6Al-4V合金的烧结。
[0027]本发明的方法可以用于例如生产包含多孔表面的金属植入物。如图1所示，描述了用于生产这种植入物的特定方法。将金属粉末、PFA和可溶解PFA的液体混合形成混合物。将混合物在一定形状的模具中压制(例如通过单轴，双轴或等静压)从而形成坯体。模具决定了植入物的形状，因此通常模具应为所需要的形状以避免或者至少减少所需要的大量机加工。通过使坯体与可溶解PFA的液体接触将PFA从坯体中除去从而形成金属骨架。可选择地，金属骨架可以被机加工和/或干燥加工以除去残留的液体。烧结金属骨架，随后可选择地进行机加工以形成多孔金属植入物。本领域技术人员知道这种植入物的合适形状和它们所要具备的性能，例如合适的压缩屈服(yield)强度。尽管图1所示的第一液体和第二液体来自于相同的来源，但是我们知道：这些液体不必是相同的，只要他们均可溶解造孔剂即可。
[0028]多孔金属植入物的表面可以被粗糙化。粗糙化的方法包括喷丸处理、酸蚀或等离子喷射中的至少一种以及为本领域已知的技术。酸蚀的优选方法是美国专利申请号为2004/0167633中所公开的酸蚀方法，整个公开的内容在这里被引用。优选的喷丸处理方法采用水溶性粒子，例如NaCl，喷向植入物，因此可以通过溶于含水的液体将已压紧的粒子从空隙中除去。
[0029]在某些具体实施例中，本发明提供孔隙度为约60％到约85％(优选约65％到约75％)的金属植入物或其它类型金属骨架，通过体积、液体水银的强制压入和剖面图分析来测量。可以理解的是：孔隙度为金属与PFA比例、PFA尺寸或者二者结合的产物。
[0030]在一个实施例中，优选的纯钛骨架是在孔隙度约为65％的情况下，具有约35MPa的抗拉强度(通过标准的拉力测试机测量-ASTM E8-99)，或者具有至少约90MPa的弯曲屈服强度(通过三点弯曲测量-ASTM E290-97a)，和/或具有至少约65MPa的压缩屈服强度(通过单向压缩测量-ASTM E9-89a)的那些骨架。特别优选的纯钛骨架是那些在孔隙度约为65％的情况下具有至少约40MPa的抗拉强度(通过ASTM E8-99测量)，或具有至少约110MPa弯曲屈服强度(通过ASTM E290-97a测量)，和/或具有至少约75MPa压缩屈服强度(通过ASTM E9-89a测量)的骨架。
[0031]可以理解的是：可以使用钛合金以得到更高的强度。优选的钛合金骨架是在孔隙度约为65％的情况下，具有约60MPa的抗拉强度(通过ASTME8-99测量)，或者具有至少约120MPa弯曲屈服强度(通过-ASTM E290-97a测量)，和/或具有至少约90MPa压缩屈服强度(通过ASTM E9-89a测量)的那些。特别优选的钛合金骨架是那些在孔隙度约为65％的情况下，具有至少约90MPa的抗拉强度(通过ASTM E8-99测量)，或具有至少约180Mpa的弯曲屈服强度(通过ASTM E290-97a测量)，和/或具有至少约为110Mpa的压缩屈服强度(通过ASTM E9-89a测量)的那些。
[0032]即使不需要受理论约束，我们也知道孔隙度、金属粉末的粒度和烧结温度是影响产物结构强度的重要因素。
具体实施例
[0033]通过以下的例子对本发明进行详细说明，但是这些例子不能用来限制本发明。
实施例1
[0034]将颗粒尺寸为45-75μm的工业纯钛粉末(Phelly材料公司，伯根菲尔德，新泽西，美国)和作为PFA的颗粒尺寸为250-425μm的NaCl(FisherScientific International公司，汉普敦，新罕布什尔州，美国)按体积比约为25∶75的Ti∶PFA的比例混合。每100cm3的Ti∶PFA的混合物中对应加入约700μL的反渗透水。将上述混合物加入到模具中并用22ksi的压力压制成坯体。再将坯体浸入到水浴器中直到NaCl溶解。将生成的金属骨架在65℃干燥4小时，然后在1204℃烧结2小时。烧结后的金属泡沫结构如图2-5所示，图中示出了非常好的具有复杂形状的多孔金属泡沫结构。
实施例2
[0035]将颗粒尺寸为45-75μm的工业纯钛粉末和作为PFA的颗粒尺寸为250-425μm的NaCl，按体积比约为20∶80的Ti∶PFA的比例混合。每100cm3的Ti∶PFA的混合物中对应加入约700μL的反渗透水。将上述混合物加入到模具中并用23.6ksi的压力压制成坯体。再将坯体浸入到水浴器中直到NaCl溶解。将生成的金属骨架先如实施例1中那样在炉子中干燥，然后在1371℃烧结3小时。烧结后的金属泡沫结构如图6-7所示。
实施例3
[0036]将钛粉(32-45μm(500-350目))和NaCl(425-500μm)按体积比约为25∶75的Ti∶PFA的比例混合。每100cm3的Ti∶PFA的混合物中对应加入约700μL的反渗透水。将上述混合物加入到模具中并用30ksi的压力压制成坯体。再将坯体浸入到水浴器中约12小时以使PFA溶解。将生成的金属骨架在1731℃烧结6小时。烧结后的金属泡沫结构的孔隙度约为65％。根据ASTM E9-89a和ASTM E290-97a通过执行标准压缩测试和三点弯曲测试测得的压缩屈服强度和弯曲屈服强度分别为82MPa和180MPa。
实施例4
[0037]将钛粉末(32-45μm(500-350目))和NaCl(250-300μm)按体积比约为25∶75的Ti∶PFA的比例混合。每100cm3的Ti∶PFA的混合物中对应加入约700μL的反渗透水。将上述混合物加入到模具中并用45ksi的压力压制成坯体。再将坯体浸入到水浴器中约12小时以使PFA溶解。将生成的金属骨架在1371℃烧结6小时。烧结后的金属泡沫结构的孔隙度约为65％。参照实施例3的上述方法测得的压缩屈服强度和弯曲屈服强度分别为77MPa和196MPa。
[0038]如前所述，已参照具体实施例对概念进行了描述。上文已经描述了本发明的很多方面和具体实施例，但它们仅仅是示例性的而不是对本发明的限定。通过阅读说明书，本领域技术人员可以认识到：其它方面和实施例并未离开本发明的范围。此外，本领域普通技术人员可以认识到：可以在不离开如在下面的权利要求书中所阐述的本发明的保护范围的情况下对本发明做出多种改变和变化。因此，说明书和附图应该当作是说明性的而不是限制性的，并且所有的这种改变在本发明的范围之内。
[0039]在上文中参照具体实施例描述了本发明的好处、其它优点和问题的解决方法。然而，可能带来的、同样的或者更显著的好处、优点、问题的解决方法和任何特征都不能被看作是对任一或所有权利要求的关键性的、必要的或必需的特征。
[0040]可以理解的是：为了清楚起见，在本文不同的实施例的内容中描述了某些特征，但是也可以将这些特征结合提供给一个实施例。相反，为了简要起见，许多特征只在一个实施例中进行了描述，但是也可以在其它实施例中分别提供这些特征或以任何补充结合的方式来提供这些特征。此外，数值范围中提到的值包括在该范围内的每一个值。

Claims (21)

1.一种方法，包含以下步骤：
将可液体提取的造孔剂与金属粉末和第一液体混合，其中造孔剂可溶解于第一液体，因此形成混合物；
压制混合物以形成坯体；以及
将造孔剂在其可溶于其中的第二液体中溶解，因此形成金属骨架。
2.如权利要求1所述的方法，其中所述第一液体是含水的。
3.如权利要求1所述的方法，其中每100cm3的所述造孔剂与所述金属粉末的混合物与约450μL到约1050μL的所述第一液体混合。
4.如权利要求1所述的方法，其中每100cm3的所述造孔剂与所述金属粉末的混合物与约600μL到约750μL的所述第一液体混合。
5.如权利要求1所述的方法，其中第一液体为反渗透水、去离子水、蒸馏水、脱氧水、软化水或含水的碳水化合物溶液。
6.如权利要求1所述的方法，其中第一液体含有至少约75％重量百分比的水。
7.如权利要求1所述的方法，其中造孔剂为氯化钠，氯化铵，氯化钙，氯化镁，氯化铝，氯化钾，氯化镍，氯化锌，碳酸氢铵，磷酸氢钠，磷酸二氢钠，磷酸二氢钾，磷酸氢钾，亚磷酸氢钾，磷酸钾，硫酸镁，硫酸钾，碱土金属卤化物，结晶碳水化合物，聚乙烯醇(PVA)，聚乙烯氧化物，聚丙烯蜡，羧甲基纤维素钠(SCMC)，聚乙二醇-聚丙烯-聚乙二醇共聚物(PEG-PPG-PEG)，或者其混合物。
8.如权利要求1所述的方法，其中造孔剂的颗粒尺寸为约200μm到约600μm。
9.如权利要求1所述的方法，其中造孔剂的颗粒尺寸为约200μm到约350μm。
10.如权利要求1所述的方法，其中造孔剂的颗粒尺寸为约350μm到约550μm。
11.如权利要求1所述的方法，其中金属粉末由钛、钴、铬、镍、镁、钽、铌、锆、铝、铜、钼、钨、不锈钢或其合金形成。
12.如权利要求1所述的方法，其中金属粉末为钛或钛合金。
13.如权利要求1所述的方法，其中金属粉末的颗粒尺寸为约20μm到约100μm。
14.如权利要求1所述的方法，其中金属粉末的颗粒尺寸为约25μm到约50μm。
15.如权利要求1所述的方法，其中金属粉末的颗粒尺寸为约50μm到约80μm。
16.如权利要求1所述的方法，其中第一液体和第二液体是相同的。
17.如权利要求1所述的方法，其中第一液体和第二液体是不同的。
18.如权利要求1所述的方法，其中第二液体是含水的。
19.如权利要求1所述的方法，其中金属粉末与造孔剂的体积比为约40∶60到约10∶90。
20.如权利要求1所述的方法，其中金属粉末与造孔剂的体积比为约25∶75。
21.如权利要求1所述的方法，进一步包括烧结金属骨架以形成多孔金属植入物，其中烧结温度范围为约2100°F到约2700°F。
CNA2008100856651A 2007-02-21 2008-02-21 多孔金属泡沫结构及其制造方法 Pending CN101250638A (zh)

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