CN1096110C - 含有钛阻挡层的焊料凸点结构及其形成方法 - Google Patents

含有钛阻挡层的焊料凸点结构及其形成方法 Download PDF

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CN1096110C
CN1096110C CN96193314A CN96193314A CN1096110C CN 1096110 C CN1096110 C CN 1096110C CN 96193314 A CN96193314 A CN 96193314A CN 96193314 A CN96193314 A CN 96193314A CN 1096110 C CN1096110 C CN 1096110C
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约瑟夫·丹尼尔·米斯
格雷钦·马耶尔克·阿德马
马克·D·克拉姆
W·鲍伊德·罗格尔斯
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Abstract

一种在具有接触焊盘的微电子器件上形成焊料凸点的方法，包括以下步骤：在器件上淀积钛阻挡层，在钛阻挡层上形成下凸点金属化层，和在下凸点金属化层上形成一个或多个焊料凸点。焊料凸点限定了被除去的下凸点金属化层暴露的部分，然后钛阻挡层的暴露的部分被除去。钛阻挡层保护下面的微电子器件不受除去下凸点金属化层的腐蚀剂的影响。钛阻挡层也可以防止下凸点金属化层在下面的微电子器件上形成残留物。因此，钛阻挡层使得下凸点金属化层很快被除去，而不会留下残留物，因而减小了焊料凸点间电短路的可能性。

Description

含有钛阻挡层的焊料凸点结构及其形成方法
本发明涉及微电子器件的制造方法和结构，特别涉及形成微电子器件的电气和机械连接的方法，以及由此方法形成的连接。
高性能的微电子器件通常使用焊料球或焊料凸点与其它微电子器件进行电互连。例如，超大规模集成电路(VLSI)芯片可以使用焊料球或焊料凸点电连接到电路板或其它下一级封装衬底上。这种连接技术也称作“控制熔塌芯片连接-C4”或“倒装芯片”技术，在这里称作焊料凸点。
在IBM开发的最初的焊料凸点技术中，焊料凸点通过夹到集成电路硅片上的阴模中的开口由蒸发形成。例如，Katz等人的U.S.专利5,234,149“Debondable Metallic Bonding Method”公开了一种带芯片接线端和金属化层的电子器件。接线端一般为铝，金属化层包括钛或铬局部粘附层，共淀积的局部铬铜层，局部可湿润铜层，和局部金和锡帽盖层。蒸发的局部铅-锡焊料层位于帽盖层上。
以电镀法为基础的焊料凸点技术也被积极地开发。电镀法对较大衬底和较小焊料凸点特别有用。在该方法中，一般通过蒸发或溅射将“下凸点金属化(under bump metallurgy)”(UBM)层淀积在具有接触焊盘的微电子衬底上。连续下凸点金属化层一般在焊盘和焊盘间的衬底上，以便焊料电镀期间允许电流通过。
带下凸点金属化层的电镀法的例子公开于Yung的U.S.专利5,162,257“焊料凸点制造方法”中，并转让给本申请的受让人。在该专利中，下凸点金属化层包含紧邻衬底和焊盘的铬层，作为可焊金属的帽盖铜层，以及铬层和铜层之间的相控的铬/铜层。焊料凸点的基层通过将焊料凸点和焊盘间的下凸点金属化层转换为下凸点金属化层的焊料和可焊组分构成的中间金属来保持。然而需要多个腐蚀周期除去相控的铬/铜层和底部的铬层。即使进行多个腐蚀周期，也很难完全除去下凸点金属化层，并可能使焊料凸点间电短路。
尽管已有以上提到的专利，但本领域仍然需要一种形成焊料凸点的方法和因此形成的焊料凸点的结构，其中在电镀焊料凸点之后，可以很容易并完全地除去下凸点金属化层的暴露部分，因而减少焊料凸点间电短路的可能性。本领域也需要一种形成焊料凸点的方法，其中当除去下凸点金属化层的暴露部分时，不必大量地钻蚀(Undercut)焊料凸点，因而减少了发生机械或电气故障的可能性。
因此本发明的目的在于提供一种改进的制造微电子器件接触焊盘的焊料凸点的方法，以及因此形成的改进的焊料凸点。
本发明的另一目的在于减少电镀焊料凸点后除去下凸点金属化层的暴露部分所需的时间。
本发明的再一目的在于减少焊料凸点间电短路。
本发明的又一目的在于减少电镀后除去下凸点金属化层的暴露部分时焊料凸点的钻蚀。
本发明的这些和其它目的通过形成下凸点金属化层之前在微电子器件上淀积连续的钛阻挡层实现。因此，下凸点金属化层可以从钛层上被选择性地除去，然后将钛层从微电子器件上除去。钛层可防止下凸点金属化层在微电子器件上形成残留物造成焊料凸点间电短路。此外，钛层可保护下面的微电子器件不受除去下凸点金属化层的腐蚀剂的影响。
根椐本发明的一个方面，形成焊料凸点的方法包括以下步骤：在带有焊盘的微电子器件上淀积钛阻挡层，在钛阻挡层上形成下凸点金属化层，然后在下凸点金属化层上形成焊料凸点。焊料凸点限定出将选择性地除去的下凸点金属化层和钛阻挡层的暴露部分。因此，电镀焊料凸点后，下凸点金属化层的暴露部分可以很快并完全地除去，而不必大量钻蚀焊料凸点或留下导致焊料凸点间电短路的残留物。
可以使用相对于焊料凸点和钛阻挡层优先腐蚀下凸点金属化层的腐蚀剂选择性地除去下凸点金属化层的暴露部分。可以使用相对于焊料凸点和留在焊料凸点下的那部分下凸点金属化层的优先腐蚀钛阻挡层的腐蚀剂选择性地除去钛阻挡层。
下凸点金属化层最好包括钛阻挡层上的铬层，铬层上的铬层和铜层的相控层，以及相控层上的铜层。在这个实施例中，氢氧化铵和过氧化氢的混合物可以用于选择性地腐蚀下凸点金属化层的铜部分；盐酸可以用于腐蚀下凸点金属化层的铬部分；以及用氟化铵缓冲的氢氟酸选择性地腐蚀钛层。
也可以在下凸点金属化层未被焊料凸点覆盖的区域上形成焊料阻挡层(dam)，最好在除去下凸点金属化层的暴露部分之前除去该焊料阻挡层。焊料阻挡层最好包括如铬或钛层等焊料不可湿润层。焊料阻挡层也可以包括焊料不可湿润层上的如铜等的焊料可湿润材料。
形成后，可以对焊料凸点进行回流焊。回流焊焊料凸点的步骤使焊料凸点和紧邻焊料凸点的下凸点金属化层的未暴露部分之间发生反应，从而产生金属间区域，其中除去下凸点金属化层的铜部分的腐蚀剂相对于金属间区域优先腐蚀铜。
图1-6为根据本发明形成焊料凸点的第一个方法的不同步骤期间，带焊盘的微电子器件的剖面图。
图7-12为根据本发明形成焊料凸点的第二个方法的不同步骤期间，带焊盘的微电子器件的剖面图。
下面结合附图更详细地介绍本发明，其中显示了本发明的优选实施例。然而，本发明可以体现为许多不同形式，不应仅局限在以下介绍的实施例中；而且，提供这些实施例是为了公开充分，使本领域的普通技术人员完全明确本发明的范围。为清楚起见，层的厚度进行了夸大。同样的元件采用了相同的数字。
如图1所示，微电子器件20包括衬底22，多个接触焊盘24，以及钝化层26。衬底22可以包括一层半导体材料，该半导体材料可以为硅、砷化镓、碳化硅、金刚石、印刷电路板或多层衬底、或本领域的普通技术人员公知的其它衬底材料。接触焊盘24可以包括铝、铜、钛、以上提到的金属的结合如AlCu和AlTi3的中间金属、或本领域的普通技术人员公知的其它材料。钝化层26最好为聚酰亚胺层，但也可以是二氧化硅层、氮化硅层、或本领域的普通技术人员公知的其它钝化材料。如图所示，钝化层最好覆盖与衬底相对的每个接触焊盘的上部边缘部分，暴露每个接触焊盘的中间的表面部分。
在微电子器件20上需要有焊料凸点以便器件可以电气地和机械地连接到如电路板等的另一个微电子器件或其它下一级封装衬底上。接触焊盘要预先处理除去任何自然氧化物，这对本领域的普通技术人员是公知的。连续的钛阻挡层28(大约500埃厚)跨越钝化层26和接触焊盘24暴露的表面形成。不必大量腐蚀钝化层就可以很容易地从钝化层26上腐蚀掉钛阻挡层28。如果使用钛接触焊盘，由于钛阻挡层可以将氧气从钛接触焊盘中吸除，所以可以省掉预处理步骤。
然后在钛阻挡层28上形成连续的下凸点金属化层。下凸点金属化层由能使焊料凸点和接触焊盘之间充分粘接的材料形成，而不必大量腐蚀钛阻挡层就可以很容易地从钛阻挡层28上腐蚀掉该材料。因此，下凸点金属化层最好包括铬层30(大约1000埃厚)，铬层上的铬层和铜层相控层32(大约1000埃厚)，以及相控层上的铜层34(大约1微米厚)。包括铬层，铬层上的铬层和铜层相控层，以及相控层上的铜层的下凸点金属化层已在，例如，Yung的U.S.专利5,162,257“焊料凸点制造方法”中讨论过，在这里作为参考引入。
形成下凸点金属化层之后，形成焊料阻挡层。在优选实施例中，焊料阻挡层包括一层不可湿润层36(大约1500埃厚)，最好为一层铬或钛。焊料阻挡层也可以包括焊料可湿润层38(大约125埃厚)，例如焊料不可湿润层36上的铜层。例如，铜层在铬层上的焊料阻挡层允许焊料镀在其上，而后来的回流焊步骤将熔解暴露铬的铜。在这个实施例中，焊料可以均匀地电镀在焊料阻挡层的焊料可湿润层38上。然后将没有被焊料覆盖的焊料可湿润层的部分除去，因此防止了回流焊步骤期间焊料凸点的膨胀。当焊料加热到它的液化温度以上时(对含95％的铅和5％的锡的焊料大约为312℃)，焊料将回流、熔解可湿润层38剩下的部分，并与不可湿润层36接触。因此，回流的焊料凸点由于表面张力将大体上形成球形。图2显示的微电子器件20包括钛阻挡层28；具有铬层30，铬和铜的相控层32，和铜层34的下凸点金属化层；具有焊料不可湿润层36和焊料可湿润层38的焊料阻挡层。钛、铬、相控的铬和铜，和铜层中的每一层都是由蒸发、溅射、或本领域的普通技术人员公知的其它淀积技术形成。铬和铜的相控层可以由铬和铜共淀积形成。
如图3所示，选择除去接触焊盘24上需要形成焊料凸点的区域内的焊料阻挡层。可以通过标准的光刻/腐蚀技术或剥离(lift-off)技术选择除去焊料阻挡层的部分。如果使用了标准的光刻/腐蚀技术，由于不必大量地腐蚀铜层就可从下面的铜层34上选择性地除去钛，所以钛可优选地用做焊料不可湿润层36。未被焊料阻挡层(层36和38)覆盖的铜层34的区域限定了回流焊步骤后微电子器件上焊料凸点的表面区域，这将在下面讨论。
如光刻胶掩模等构图的掩模层40也形成在焊料阻挡层上，限定了焊料阻挡层和焊料要电镀的下凸点金属化层上未覆盖的区域。如图3和4所示，掩模层40未覆盖的表面区域大于焊料阻挡层(层36和38)未覆盖的各自的表面区域，因而可在更大的区域上镀焊料。如图4所示，焊料凸点42电镀在掩模层40未覆盖的区域上。
使用本领域的普通技术人员公知的电镀技术将焊料镀在焊料阻挡层和下凸点金属化层上未覆盖的区域。例如，带掩模层40的微电子器件20表面暴露在含有铅和锡的镀液中，偏置电压施加到包括铬层30，铬和铜的相控层32，和铜层34的连续的下凸点金属化层上。如图4所示，偏置电压使铅-锡焊料镀在铜层34和38的未覆盖部分上形成焊料凸点42。
通过控制掩模层40未覆盖的区域、施加的偏置电压、镀液的浓度，和电镀步骤的持续时间可以控制电镀的焊料量。由于焊料不能均匀地镀在如铬等焊料不可湿润材料上，在焊料不可湿润层36上使用带如铜层等的焊料可湿润层38的焊料阻挡层可使焊料均匀地镀在焊料阻挡层上未被掩模层覆盖的区域内。因此，焊料要电镀的区域，和所得的电镀量的决定都与焊料阻挡层未覆盖的区域无关，而焊料阻挡层未覆盖的区域决定了回流焊后微电子器件上焊料凸点的表面区域。
如图5所示，完成电镀步骤后，除去掩模层40和未被焊料凸点覆盖的焊料可湿润层38，之后将焊料凸点42加热到液化温度(对含95％的铅和5％的锡的焊料大约为312℃)以上，以使它们回流。如果焊料可湿润层为铜层，那么氢氧化铵和过氧化氢的混合物可以除去焊料可湿润层。当焊料凸点电镀到焊料阻挡层的焊料可湿润层38处，焊料可湿润层38熔解到焊料凸点中暴露焊料不可湿润层36于焊料凸点。因此，表面张力使回流的焊料凸点42在下凸点金属化层上未被焊料阻挡层覆盖的部分上大体上形成球形。当焊料凸点冷却时，固化的焊料保持大体上的球形。
此外，回流的焊料在紧邻焊料凸点的下凸点金属化层的部分形成金属间区域34′。在优选实施例中，下凸点金属化层包括铬层30，铬和铜的相控层32，和铜层34；焊料与铜层34的部分发生反应形成金属间区域34′。这个金属间区域包括不与腐蚀剂充分反应通常用于除去铜、铬，和钛的Cu3Sn。
如图5所示，回流的焊料凸点42限定了下凸点金属化层暴露和未暴露的部分。因此，焊料凸点42可用于掩蔽支持焊料凸点的下凸点金属化层的部分。如图6所示，除去由焊料凸点暴露的下凸点金属化层的部分，以便每个焊料凸点42与其它焊料凸点电隔离。
首先有必要除去焊料不可湿润层36。如果不可湿润层为铬，可使用盐酸除去焊料不可湿润层。同样，如果钛被用做不可湿润层，可使用氟化铵缓冲的氢氟酸除去。
焊料凸点42暴露的下凸点金属化层的部分可从钛阻挡层28上有效地除去，而钛阻挡层可以保护下面的钝化层26和接触焊盘24。然后使用不会严重影响将下面的钝化层的腐蚀剂除去钛阻挡层暴露的部分。
例如，使用如氢氧化铵和过氧化氢的混合物的化学腐蚀剂可以腐蚀由焊料凸点42暴露的铜层34。相对于焊料凸点、钛阻挡层28，和金属间区域34′，该混合物优先腐蚀铜层。因此，该腐蚀不会大量减少焊料凸点的焊料量或大量地钻蚀焊料凸点。该混合物也从铬和铜的相控层32上除去一些铜。
如盐酸等的化学腐蚀剂用于腐蚀焊料凸点暴露的相控层32和铬层30剩下的部分。相对于焊料凸点、钛阻挡层，和金属间区域34′，该酸优先腐蚀相控层和铬层。该酸从钛阻挡层上除去剩下的下凸点金属化层暴露的部分而不会留下大量的残余物。
使用如氟化铵缓冲的氢氟酸等的钛腐蚀剂腐蚀焊料凸点42暴露的钛阻挡层28的部分。相对于焊料凸点42、金属间区域34′、铬和铜的相控层32，铬层30，该酸优先腐蚀钛。如果使用聚酰亚胺层做钝化层26，该酸不会大量腐蚀钝化层。如果使用二氧化硅层或氮化硅层做钝化层，该酸对钝化层有一定程度的腐蚀。可通过限制除去钛阻挡层所需的持续时间将这些材料的腐蚀减到最小。因此，聚酰亚胺层为钝化层的优选材料。最终的焊料凸点结构显示在图6中。
没有钛阻挡层，回流焊步骤后很难完全除去下凸点金属化层，并且不需要的导电残留物会残留在微电子器件上。申请人理论上认为下凸点金属化层与钝化层反应在两层的界面上形成导电反应物。如不钻蚀焊料凸点或减少焊料凸点的量，该导电反应物很难腐蚀掉，因而导致存有不希望的导电残留物。这些残留物导致焊料凸点间的电短路。
使用钛阻挡层可将回流焊步骤后的下凸点金属化层有效地除去，从而减少形成焊料凸点间电短路的残留物发生。钛阻挡层可防止凸点金属化层与钝化层发生反应因而减少残留物。然后将钛阻挡层从钝化层上腐蚀掉不会留下显著的残留物。
尽管要在结构上产生附加层，但消除不希望的残留物一般会减少除去焊料凸点间的导电层所需的时间。由于钛阻挡层减少了总的腐蚀时间，因而减少了焊料凸点暴露在腐蚀剂中的时间，钻蚀减少。附加的钛阻挡层也会增加生产成品率并减少器件发生故障的可能性。根据以上介绍的方法形成的焊料凸点还具有低电阻。例如，微电子器件上直径为50μm具有圆形表面的焊料凸点显示的电阻大约为3毫欧姆。
以上相对于图1-6讨论的方法的变形显示在图7-12中。图7显示的包括衬底22，接触焊盘24，以及钝化层26的微电子器件20已在图1中介绍过。图8显示的附加的钛阻挡层，和包括铬层30、铬和铜的相控层32，和铜层34的下凸点金属化层也已在图2中介绍过。然而，在图8中，焊料阻挡层50仅包括单个焊料不可湿润层，该层最好为钛层(大约1000埃厚)。
使用钛焊料阻挡层在图9显示的焊料凸点形成期间用一次掩模法就可完成。这里，如光刻胶掩模或本领域的普通技术人员公知的其它掩模等的掩模层52在形成焊料阻挡层50的图形之前构图。然后使用掩模层52形成焊料阻挡层50的图形。因此，仅用一次光刻步骤就可以形成掩模层和焊料阻挡层的图形。最好用钛层做焊料阻挡层，是由于可使用相对于铜和焊料优先腐蚀钛的如氟化铵缓冲的氢氟酸等的腐蚀剂从铜层34上选择性地除去钛。由于焊料未镀在焊料阻挡层上，所以焊料阻挡层50不必有焊料可湿润层。这里，焊料阻挡层50仅在回流焊步骤期间防止焊料凸点的扩展。
如图10所示，掩模层52和焊料阻挡层50限定了焊料要镀在下凸点金属化层上的区域。除了焊料未镀在焊料阻挡层上以外，电镀步骤与根据图4介绍的电镀步骤一样。电镀焊料凸点之后，选择性地除去掩模层40，并且将焊料凸点加热到液化温度(对含95％的铅和5％的锡的焊料大约为312℃)以上回流焊料。焊料阻挡层50可防止回流的焊料流到要求的区域以外。如图11所示，表面张力使回流的焊料54形成大体上的球形。当焊料凸点冷却时，焊料凸点固化并保持这种形状。和以上讨论的图5一样，回流步骤也用于在铜层34中形成金属间区域34′。
和以上讨论的图5和6一样，焊料凸点限定了下凸点金属化层和钛阻挡层的暴露和未暴露的部分，除去暴露的部分，以便如图12所示使每个焊料凸点电绝缘。首先将焊料阻挡层50用如氟化铵缓冲的氢氟酸等的腐蚀剂除去。然后和以上讨论的图5和6一样，除去下凸点金属化层和钛阻挡层。
在图和说明书中，已公开了发明的一般优选实施例，虽然使用了特定的术语，但为一般的和说明性的理解，而不是为了限定，本发明的保护范围由以下权利要求限定。

Claims (10)

1.一种在微电子器件(20)上形成焊料凸点(42)的方法，微电子器件(20)具有衬底(22)和所述衬底(22)上的多个接触焊盘(24)，其中每个所述接触焊盘(24)都有暴露的表面部分，所述方法的特征在于以下步骤：
在所述接触焊盘(24)上形成连续的钛阻挡层(28)，其中所述阻挡层(28)覆盖所述接触焊盘(24)的所述暴露的表面部分，并在所述衬底上延伸；
在面对所述衬底的所述阻挡层(28)上形成下凸点金属化层(30，32，34)；
在面对所述接触焊盘(24)中的一个和所述阻挡层的所述暴露的表面部分，在所述下凸点金属化层(30，32，34)上形成焊料凸点(42)，因而限定了所述下凸点金属化层上暴露的和未暴露表面部分；
选择性地除去所述下凸点金属化层(30，32，34)的所述暴露部分，因而限定了所述阻挡层(28)的暴露部分；
选择性地除去所述阻挡层(28)的所述暴露部分；并且
其中形成下凸点金属化层的步骤包括：
在所述钛阻挡层(28)上形成铬层(30)，和
在面对所述阻挡层(28)的所述铬层(30)上形成铜层(34)。
2.根据权利要求1的方法，其中形成下凸点金属化层的所述步骤还包括：
形成所述铜层之前在面对所述阻挡层的所述铬层上形成铬和铜的相控层。
3.根据权利要求1的方法，其中在所述下凸点金属化层的所述暴露部分上形成包括焊料不可湿润层的焊料阻挡层的步骤先于所述形成焊料凸点的步骤，其中除去所述焊料阻挡层的步骤先于所述选择性地除去所述下凸点金属化层的所述暴露部分的步骤。
4.根据权利要求2的方法，其中所述选择性地除去所述下凸点金属化层(30，32，34)的所述暴露部分的步骤还包括：
对所述铜层(34)的所述暴露部分使用铜腐蚀剂，其中相对于所述焊料凸点(42)、所述铬层(30)、和所述钛阻挡层(28)，所述铜腐蚀剂优先选择性地腐蚀所述铜层(34)和所述相控层(32)的所述铜部分；以及
对所述相控层(32)的所述铬部分和所述铬层(30)使用铬腐蚀剂，其中相对于所述焊料凸点(42)、所述铜层(34)、和所述钛阻挡层(28)，所述铬腐蚀剂优先选择性地腐蚀所述相控层(32)的所述铬部分和所述铬层(30)。
5.根据权利要求3的方法，其中所述形成焊料阻挡层的步骤还包括在面对所述下凸点金属化层上的所述焊料不可湿润层(36)上形成焊料可湿润层(38)的步骤。
6.一种微电子器件(20)的焊料凸点结构，微电子器件(20)具有衬底(22)和所述衬底(22)上的多个接触焊盘(24)，其中每个所述接触焊盘(24)都有面对所述衬底的暴露的表面部分，所述焊料凸点结构的特征在于：
连续的钛阻挡层(28)在所述衬底上延伸并与所述每个接触焊盘(24)所述的暴露的表面部分接触；
在面对所述衬底的所述阻挡层(28)上形成连续的下凸点金属化层(30，32，34)；
在面对所述接触焊盘(24)中一个的所述下凸点金属化层(30，32，34)上形成焊料凸点(42)；并且
其中所述连续的下凸点金属化层包括：
在所述钛阻挡层(28)上的铬层(30)，
在相对于所述阻挡层(28)的所述铬层(30)上的铜层(34)。
7.根据权利要求6的焊料凸点结构，其中所述连续的下凸点金属化层还包括：
在所述铬层和所述铜层之间的铬和铜的相控层。
8.根据权利要求6的焊料凸点结构，其中所述焊料凸点限定了所述下凸点金属化层的暴露部分，所述结构还包括：在面对所述阻挡层的所述下凸点金属化层的所述暴露部分上的焊料阻挡层，并且其中所述焊料阻挡层包括焊料不可湿润层。
9.根据权利要求8的焊料凸点结构，其中所述焊料不可湿润层(36)选自包括钛层和铬层的组中。
10.根据权利要求8的焊料凸点结构，其中所述焊料阻挡层还包括相对于所述下凸点金属化层，在所述焊料不可湿润层(36)上的焊料可湿润层(38)。
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EP1441388A3 (en) 2004-09-22
US5767010A (en) 1998-06-16
ATE210895T1 (de) 2001-12-15
KR100367702B1 (ko) 2003-04-07
KR19980703139A (ko) 1998-10-15
AU6376796A (en) 1996-10-16
WO1996030933A3 (en) 1996-11-28
HK1036523A1 (zh) 2002-01-04
EP0815593A2 (en) 1998-01-07
WO1996030933A2 (en) 1996-10-03
DE69617928D1 (de) 2002-01-24
ATE271718T1 (de) 2004-08-15
EP1441388A2 (en) 2004-07-28
DE69632969D1 (de) 2004-08-26
US6222279B1 (en) 2001-04-24
EP0815593B1 (en) 2001-12-12
EP1134805B1 (en) 2004-07-21
EP1134805A3 (en) 2001-12-12
DE69632969T2 (de) 2005-07-28
CN1181841A (zh) 1998-05-13
EP1134805A2 (en) 2001-09-19
DE69617928T2 (de) 2002-07-18
JPH11505668A (ja) 1999-05-21

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