CN88102545A - 多层超导电路衬底及其制备方法 - Google Patents

多层超导电路衬底及其制备方法 Download PDF

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CN88102545A
CN88102545A CN88102545A CN88102545A CN88102545A CN 88102545 A CN88102545 A CN 88102545A CN 88102545 A CN88102545 A CN 88102545A CN 88102545 A CN88102545 A CN 88102545A CN 88102545 A CN88102545 A CN 88102545A
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biscuit
superconducting ceramics
ceramics
metallic paint
superconducting
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今中佳彦
町敬人
山中一典
横山博三
龟原伸男
丹羽纮一
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Fujitsu Ltd
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Abstract

本发明提供了一种多层超导电路衬底，它包括绝缘层和位于绝缘层之间的超导陶瓷材料的内连接模块，借助于超导陶瓷材料通孔将超导陶瓷材料模块连通。超导陶瓷材料的模块最好用金、银、铂及其合金封装。

Description

本项发明所涉及的是多层超导电路衬底，特别是适合于高速计算机如超大型计算机上使用的多层超导电路衬底及其制备工艺。使用在高速作业中的衬底，即要求衬底上的导电材料具有低电阻，又要求衬底上的绝缘材料具有低介电常数，以确保信号的有效传递。
用玻璃-陶瓷材料，即陶瓷和玻璃的复合材料（介电常数ε≈5）作为绝缘材料，用铜（电阻率为
Figure 88102545_IMG2
＝1.7Ω·cm）作为导电材料，组成多层陶瓷衬底，这称之为高速作业衬底（例如，参见Yogyo Kyokai年会文集，1985年，第533页）。
日本免检专利第60-173885号，发表于1985年11月7日，描述了超导氧化物材料BaBiO3-6（0≤δ＜0.5），其中低于50%的钡原子可由Sr、Pb、Sc、Y或某种镧系元素替换，该种超导氧化物材料的超导转变温度约为12k，同时该专利还描述了制备超导氧化物材料BaBiO3（0 δ＜0.5）工艺。工艺包括：将Ba和Bi的两种化合物均匀地混合，在高于600℃温区的氧化气氛中煅烧混合原料;粉化煅烧过的坯体;将生成的粉末压成体材;在700℃温区高于10kg/cm2的氧压气氛中退火，以补偿煅烧时损失掉的大量氧成分。
业已知道如下的氧化物超导材料：
（1）La-Bg-Cu-O系列：
参考文献：
Bednorz：瑞士物理B（Z.Phys.B）1986年64卷等第189页;
Uchida：日本应用物理杂志（J.J.A.P）1987年26卷第一期L1;
Chu：物理评论通讯（Phys    Rev.lett）1987年58卷第四期第405页
Jorgensen：物理评论通讯（Phys    Rev    lett）1987年58卷第十期1024页
（2）La-Sr-Cu-O系列
Cava：物理评论通讯，1987年58卷第四期408页
Mattheiss：物理评论通讯（Phys    Rev    lett）1987年58卷第十期1028页
（3）Y-Ba-Cu-O系列
Hor：物理评论通讯（Phys    Rev    lett）1987年58卷第九期911页;
Wu：物理评论通讯（Phys    Rev    lett）1987年58卷第九期908页。
具体地说
（1）La-Ba-Cu-O系列包括
Figure 88102545_IMG4
（2）La-Sr-Cu-O系列包括
La1.9Sr0.1CuO4
La1.8Sr0.2CuO4：Tcf＝28.5K，Tcm＝33.1K，
Tco＝36.5K
La1.7Sr0.3CuO4：Tcm＝15K，Tco＝35K
La1.925Sr0.075CuO4：Tcf＝26.5K，Tcm＝34K
Tco＝52K
La1.85Sr0.15CuO4：Tcf＝36K，Tcm＝37.5K，Tco＝40K
（3）Y-Ba-Cu-0系列包括
（Y0.6Ba0.4）2CuO4：Tcf＝88.5K，
＞77K，Tco≥100K
Y-Ba-Cu-O（由Keiichi    Ogawa制备）
Tcf＝77K，Tco＝100K
Y-Ba-Cu-O（由分子研究所和Tohoku大学制备）
Tc＝95K
Y0.4Ba0.6CuO3（由Kazumaza Togano制备）
Tcf＝93K，Tco＝123K
目前利用在衬底上的导电材料具有电阻，这禁止了更细更长的内连接模式的设计。因此对高速作业的衬底是有要求的，只有导电材料具有更低的电阻衬底，才会使用在下一代计算机中。虽然超导氧化物材料符合这项要求，即更低的电阻，但是把超导氧化物材料制成内连接模式是困难的。因为模式图线的密度将做得较高，新的内连接模式图线应该有确定的边界面，至少是和铜的模式图线一样确定，以便减少相邻连线间的相互作用。
本项发明的目的是提供含有低电阻和确定边界面的导电模式图线的多层衬底。
多层衬底包括：多层衬底内分开的多个绝缘层;绝缘层具有贯穿该层的孔;在绝缘层之间的超导陶瓷材料的内连接层;超导陶瓷材料填满绝缘层上的通孔使各内连接层之间电连通。由此实现本项发明的上述目的和另一些目的。
这就是说，以前的在多层衬底上的铜内连接模式技术现在由超导陶瓷材料如包括Y-Ba-Cu-O，La-Sr-Cu-O和Sc-Ba-Cu-O系列的氧化物超导材料的内连接模式所取代。这些氧化物超导材料在氮的沸点以上，即77K以上呈现出超导电性。
在本项发明中，所利用的典型陶瓷超导材料是氧化物陶瓷材料，可用一般分子式XaY1-aZOb或（X1-aYa）2ZOb表示，这里0＜a＜1;3＜b＜4;X是Ba、Ca、Sr和Mg族选出的至少一个元素，Y表示从Sc、Y、La、Ce、Pr、Nb、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb和Lu中选出的至少一个元素;而Z是从Cu、Ag和Au中选出的至少一个元素。
上述公式中的X、Y、Z可以是多种元素。例如，X可以是Ba-Ca-Sr，Ba-Ca-Mg，Ba-Ca，或者Ca-Mg;Y可以是Sc-Y，Sc-Y-La，Sc-Y-La-Ce，或者Pr-Nb;而Z可以是Cu-Ag，Cu-Au，Ag-Au，或者Cu-Ag-Au。
这样，氧化物超导材料可以为：
例如：
（Ba0.6Ca0.2Sr0.2）0.6（Sc0.7Y0.2La0.1）0.4（Cu0.8Ag0.2）3O4-δ
或者（Ba0.8Mg0.2）0.7（Sc0.6Nd0.4）0.3Cu3O4-δ
优先选用的氧化物超导材料是：｛（MⅡO）x（MⅢ 2O3）1-x｝y-（CuO）z（O）8，这里MⅡ表示至少是Ba、Sr、Ca和Mg元素中的一个;MⅢ表示至少是Y、Sc、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Tb和Lu元素中的一个;0.5≤X≤0.9;1≤Y≤2;1≤Z≤2;而δ表示氧含量与理想化学配比的偏离;氧化物超导材料在氮的沸点以上就可呈现超导电性。
超导陶瓷材料的另一个实例是铋系（Bi-Sr-Ca-Cu-O系列）超导陶瓷材料。铋系列超导陶瓷材料的准确化学式目前尚无所知，但是它可从Bi、Sr、Ca和Cu化合物按0.25-2∶0.1-5∶0.1-5∶0.5-4的摩尔比（以这些元素为基础）混合作为原材料而制备出来。例如，1∶1∶1∶2;1∶1∶1∶3;4∶3∶3∶6;和4∶3∶3∶4。更进一步另外的超导陶瓷材料可以从Tl、Bi、Sr、Ca和Cu的化合物按0.25-2∶0.25-2∶0.1-5∶0.1-5∶0.5-4的摩尔比（这上述元素为基满）混合作为原材料而获得。这些超导陶瓷材料在氮的沸点（77K）以上呈现超导电性。
在优先选择的具体装置中，超导陶瓷材料的内连接层是由金、银、铂或它们的合金中挑选的金属包封起来的，以防止超导陶瓷材料和夹着它的上、下绝缘层中的绝缘材料在绝缘材料素坯的加热或超导材料的退火过程中发生反应。在加热或退火过程中超导陶瓷的配料会扩散进入到绝缘材料中。超导陶瓷材料和绝缘材料间的反应或者超导陶瓷材料的配料向绝缘材料内扩散会引起超导陶瓷材料的超导电性的破坏。由于金、银、铂其及它们的合金能够承受含氧气氛下1000℃的高温加热或退火，所以超导陶瓷层的包装反应该是金、银、铂及其合金这类贵金属。在含氧气氛下大约1000℃温区内维持或恢复超导陶瓷材料的超导电性是必需的，这些金属还可以增加陶瓷超导模式线的电导率。
多层衬底绝缘层中的绝缘材料最好取玻璃/陶瓷复合材料，它由玻璃/陶瓷的素坯在低于超导陶瓷材料的退火温度下烧结而成。如果从素坯烧结绝缘材料的温度过高，超导陶瓷材料在绝缘材料的素坯加热过程中其超导电性降低。这种玻璃/陶瓷复合体，即陶瓷和玻璃的复合材料的一个实例是：其组分为20%到50%的氧化铝重量，10%到60%的石英重量，20%到40%的玻璃或结晶化玻璃重量;在低于加热超导陶瓷材料涂料的温度下烧结而成，其温度的典型值为低于1000℃，最好取900℃以下。
本项发明的另一方面是提供加工多层衬底工艺，该工艺包括：准备绝缘材料素坯;在每块素坯上制备超导陶瓷材料的内连结模块;制出贯穿素坯的超导陶瓷材料通孔;把具有内连结模块和通孔的素坯层层叠放并加压，加热该层压制件，通过上述步骤，包括有绝缘材料层，超导陶瓷材料内连接模式图线以及超导陶瓷材料通孔的多层衬底就成形了。
在本项发明所优先选择的具体装置中，提供了加工多层衬底的工艺，其步骤包括：准备绝缘材料的素坯;素坯有第一和第二主表面并有孔穿透它;在每块素坯的第一和第二主表面上加上金属涂料，金属涂料复盖素坯上穿透孔的内表面;金属涂料的金属是从金、银、铂及其合金中选取的;在金属涂料上和金属涂料内制成超导陶瓷材料涂料的内连接模式。超导陶瓷材料涂料要填满穿透孔，具有金属涂料和超导陶瓷涂料的素坯层层叠上加压，此时超导陶瓷材料的内连接模式就用金属涂料包住了，而且和素坯隔开;加热该层压制件，可获得包括绝缘层和由金属包封的超导陶瓷材料内连接模式在内的多层衬底。
进一步，本项发明为通过刷制和加热方法制备超导陶瓷薄膜提供了一种涂料，涂料组成为：超导陶瓷材料粉末或者加热后才能形成超导陶瓷材料的各种配料粉末;有机粘合剂;和不易挥发的溶剂。一般说，涂料由100份上面所说的无机粉末;0.5到10份的有机粘合剂;和5到10份的不易挥发的溶剂组成的。
图1是例子1中的多层衬底制备工艺流程图;
图2A和2B是例子1中的多层衬底剖面图;
图3给出了在例子1中的多层衬底内超导陶瓷材料模式的电阻率;
图4是例子2中的多层衬底制备工艺流程图;
图5是例子2中在层叠之前素坯的剖面图;
图6是例子2中多层衬底剖面图;
图7是例子2中另一个多层衬底剖面图;
图8是粉化超导陶瓷材料工艺的草图;
图9是通过生成球穿透例4的素坯而在素坯中形成通孔的主要步骤的说明图解;
图10是将集成电路安装在多层衬底上的电子器件的透视图。
例1
本项发明的第一个具体装置描述是以图1的工艺流程图和图2的多层衬底剖面图为基准的。
超导陶瓷材料的涂料是将BaCO3，Y2O3和CuO的配料粉末按0.6∶0.2∶1的摩尔比混合，并把这种颗粒粉末球磨20小时以使之形成均匀的混合物。在200MPa的大气压下把这种混合物压成具有30mm直径的圆片。然后，该圆片在900℃的通空气条件下进行6小时热处理，并粉末化形成Ba0.6Y0.4CuO4-δ的颗粒粉末。在Ba0.6Y0.4CuO4-δ的颗粒粉末中加入粘合剂（如乙（烷）基纤维素），品醇和丁酮，然后在混合体中搅拌大约十分钟，再经过三十分钟滚磨，这是第二次搅拌。这样合成涂料具有2000泊的粘度性。
超导陶瓷材料可以是前面提到的Y-Ba-Cu-O系统，Sc-Ba-Cu-O系统或La-Sr（Ba）-Cu-O系统。优先选择的是Y-Ba-Cu-O超导陶瓷材料系统，如YBa2Cu3O7-δ，Y0.4Ba0.6CuO3或（Y0.6B0.4）2CuO4-δ这些材料在液氮温度都显示出超导电性。粘合剂可以是任何有机粘合剂，但乙基纤维素，聚乙烯丁醇，甲基纤维素，丙烯酸基聚合物等是被优先考虑的。
玻璃陶瓷材料的素坯按如下的方式制备：把具有平均颗粒度大约为3μm的氧化铝和玻璃粉末颗粒，粘合剂和溶剂混合在一起并球磨搅拌30小时。合成的粘合填充料利用流延法做成干厚大约为300μm的素坯，玻璃陶瓷素坯的厚度最好在100-500μm，当然200-300μm厚度更好。素坯切成150mm×150mm方块，切好的素坯进行穿眼打孔以便用来作通孔。
素坯或绝缘材料的组份如下，正如1984年6月6日发表于“日本国免检专利公报（Kokai）”第59-955号专利所给出的。
玻璃陶瓷粉末颗粒的组份（重量百分比%）
Al2O350.5
SiO235.0
B2O313.0
N2O 0.75
K2O 0.70
CaO    0.15
Li2O 0.15
玻璃陶瓷涂料的组份（重量百分比%）
玻璃陶瓷粉末    57.8
聚甲基丙烯酸盐树脂    8.7
双丁基钛（增塑剂）    4.6
丁酮    16.1
甲醇    溶剂    8.7
丁醇    2.9
从具有以上组份的涂料出发，一个具有均匀厚度，如0.3mm的素坯可利用流延法制得。另外，此种涂料可用作印刷涂料。
还有一种玻璃陶瓷可以使用，它是由20%-50%重量百分比的氧化铝，10%-60%重量百分比的石英玻璃和20%-40%重量百分比的玻璃或结晶玻璃混合组成，它可在比超导陶瓷材料烧结温度低的温度下烧结，即低于1000℃（“日本国免检公报（Kokai）”第60-254697号，1985年12月16日发表）。这种复合材料的一个例子是具有如下的玻璃陶瓷粉末和涂料组份。
玻璃陶瓷粉末组份（重量百分比%）
Al2O334.2
SiO259.3
B2O34.9
Na2O 1.3
K2O 0.2
CaO    0.1
玻璃陶瓷涂料的组份（重量百分比%）
氧化铝    19.8
石英玻璃    19.8
硼硅玻璃    19.8
聚甲基丙烯酸盐酯系统树脂    5.9
双丁基酞（增塑剂）    2.2
丁酮    32.5
这种浆料可用流延法形成素坯或用作印刷的绝缘涂料。
一种内连接模式的陶瓷超导材料涂料刷在合成的素坯上，其厚度大约为20μm。这种陶瓷超导材料的涂料可以由BaCO3，Y2O3和CuO粉末按0.6∶0.2∶1的摩尔比混合，再加上粘合剂，品醇和丁酮所制成的涂料替代。陶瓷超导材料的内连接模块的厚度最好大于20μm，当然20μm至40μm之间更好。利用相同的刷制步骤或分离步骤，陶瓷超导材料的涂料也可填满在素坯的孔中以形成电通孔。
将三十片这种干燥的刷制素坯层叠起来在30MPa大气压下压紧。这种压片制件在1000℃空气气氛下烧5小时以形成由固结的玻璃-陶瓷绝缘层和陶瓷超导层所组成的多层衬底。烧结气氛可以是氧气氛，也可是低于一大气压的低压氧气氛。然后把得到的多层衬底放入900℃氧气氛中退火30分钟。
图2A显示了所得的多层衬底1，其中多重玻璃-陶瓷绝缘层2被压实，超导陶瓷层，即模式3，插入到绝缘层2之间，并通过通孔4与近邻的陶瓷超导层，即模式3，内连接。由图2A可见，附加绝缘层5可被插入到绝缘层2之间，在此不存在超导陶瓷模块（片），如果必要的话，这一过程可利用屏蔽印刷方法完成。
用四极探针方法测量了这种多层衬底的电阻，结果表示在图3中。电阻在液氮温度77K时下降到零。
一种与上面相似的多层衬底可以在坚实的或烧成的陶瓷基底象氧化铝板上形成。图2B给出了这样的多层衬底。利用屏蔽印刷方法把超导陶瓷材料3和绝缘材料2的涂料层逐次地，重复地刷在氧化铝板b上，尔后烧结，这样利用厚膜制备方法以氧化铝板作为基底的多层衬底就制得了。
例2
如下的描述是参照图4，图5和图6所作的。
超导陶瓷材料涂料的准备过程与例1的相同。
把平均颗粒尺寸大约为1μm的黄金颗粒粉同粘合剂，萜品醇和丁酮混合在一起并搅拌大约10小时形成涂料混合物，在这期间丁酮完全蒸发掉，以得到黄金涂料。作为第二次搅拌，上次搅拌后的混合物经过30次的滚磨之后，可得粘性大约2000泊的黄金涂料。如果合成的黄金涂料具有高于2000泊的粘性，可加入少量的品醇以使粘性下降到2000泊左右。
玻璃陶瓷材料素坯的制备过程与例1的相似。在具有通孔的150mm×150mm见方素坯准备好以后，黄金涂料的第一模型12刷在第一个素坯11的表面上。黄金涂料的干层厚小于10μm较合适，最好是5到10μm。黄金涂料模块具有第一模块12，它对应于超导陶瓷材料的第一内连接模块13并且具有的模块宽度大于超导陶瓷材料第一内连接模块13的宽度，比如，黄金涂料的第一模块12的宽度在100μm到200μm之间。在刷黄金涂料时，黄金涂料被灌入到第一素坯11的孔中并覆盖住孔的内表面，形成黄金层14，进入孔中的黄金涂料消耗量可通可调整黄金涂料的粘性来控制，不管怎样，由黄金涂料覆盖的内表面会受处理过程影响，如果必要的话，可以把它从刷制的第一次黄金涂料模块12分离到素坯11的上表面。然后，让黄金涂料的第一模块12和黄金层14在80℃干燥10分钟。
随后，第一内连接层，即超导陶瓷材料涂料模块13在黄金涂料模块的上面和内部形成。模块13厚度大于20μm合适，最好是20到40μm，并且其宽度窄于第一黄金模块12，一般情况是50μm到150μm，比如，100μm。超导陶瓷材料涂料填满素坯11的孔中以形成通孔15。
优先把与素坯11的绝缘材料相同的涂料刷制在第一素坯11上，这里不形成黄金涂料的第一模块12。形成的绝缘材料涂料模块在图5中用参考16表示。再把黄金涂料沿着第一黄金模块12的外围边界刷制，这样超导陶瓷材料涂料模块13同绝缘材料涂料模块12就隔离开了。这附加的黄金涂料块在图5中用参考数17表示。这些黄金模块16和17是优先的，它们位于印刷素坯的表面上并与其表面对齐而不包含在素坯中。
现在来看一看第二素坯11′，第二黄金涂料模块12′和14′，第二超导陶瓷材料内连接块13′，超导陶瓷材料的通孔15′，补偿绝缘涂料模块16′和附加黄金模块17′在上表面和在第二素坯的孔中形成，其过程与第一素坯11的相同。不管怎样，第二素坯11′下表面的黄金涂料模块18需在超导陶瓷材料涂料填满孔之前印刷上。黄金涂料模块18对应于第一黄金涂料模块12，这样，当第二素坯11′叠放在第一素坯11之上时，黄金涂料模块18和12，以及17就包封了超导陶瓷材料的第一内连接模块12。绝缘材料涂料的补偿模块19可被优先地印刷在第二素坯11′的下表面上，并与其表面对齐。
与第二素坯11′的制备方式相同，包括第一素坯在内的总共30片素坯以及送够的金涂料模块，超导陶瓷材料涂料模块和绝缘材料模块被提供。
这30片素坯在30MPa大气压下层叠压片成形。图6是合成层压制件的剖面图，其中数21标记绝缘素坯，22标记超导陶瓷材料模块，23标记金料模块，24标记绝缘材料模块（或层）。在图6中，超导陶瓷材料涂料模块25和26被绝缘材料涂料模块28隔离，同时超导陶瓷材料涂料模块26和27通过金料模块29而连接起来，而不是由超导陶瓷材料涂自身来连接。这后一种结构可以根据需要而改变。
然后，图6所示的层压制件在1000℃的空气气氛中烧结5小时以形成多层衬底，在这一衬底中绝缘层，金层和超导陶瓷材料层构成了独石结构。尔后，层压制件在900℃的氧气氛中退火30分钟。烧结工艺应满足使绝缘材料（此例中的玻璃和陶瓷材料）烧成并且超导陶瓷材料模块呈现出超导电性以便成电流通路。一般地，YaY1-aZOb或（X1-aYa）2ZO超导陶瓷材料要求在含氧的气氛中，如在空气气氛或在氧气氛中850℃到1000℃温区内，典型温度是950℃，进行烧结1到30小时，通常是5到12小时。烧结以后，最好在800℃到900℃的氧气氛中退火10到120分钟，通常是30分钟。
铋系统超导材料象BiSrCaCu2Ox要求在含氧的气氛中，通常是在空气中，850℃到900℃，通常是870℃到880℃温区内进行烧结1到30小时，通常是12小时。如果超导陶瓷材料的烧结和退火温度太高，材料的超导特性就会退化，甚至失去。因此，素坯绝缘材料必须能在低于超导材料烧结或退火温度下烧成，即最好的玻璃陶瓷材料是能在相对低的温度下烧成的。层压制件的烧结气氛可以是空气气氛，含氧量不低于5%的气氛，氧气氛等。
利用四极探针方法测量了所获得的多层衬底的电阻，其结果与例1的相似，见图1，在液氮温度（77K）电阻下降到零。
黄金可被其它贵金属代替，如银、铂或其合金，因为这些金属在1000℃左右的含氧气氛中是不活跃的并且作为阻挡层阻止超导陶瓷材料配料扩散进入玻璃绝缘材料中，比如，在1000℃左右的含氧气氛下铜被氧化形成氧化铜，它不能阻止超导陶瓷材料的扩散。超导陶瓷材料对玻璃陶瓷材料敏感。如果超导陶瓷材料的组份扩散到玻璃陶瓷中，超导陶瓷材料就退化且其超导电性可能失去。因此在多层衬底中最好是使用贵金属，象金、银、铂或其合金包封住超导陶瓷材料的模块。
包封超导陶瓷材料的金属可以起补偿传导模块的作用，因为象金等金属都具有高的导电性。当补偿导电模块是需要的，而超导陶瓷材料的包封是不需要的时候，金属层仅仅连接超导陶瓷材料的一面即可，即没有必要包封住超导陶瓷材料模块。
回到图5，金料模块18不在素坯11′或11″的第二表面上形成，而在第一块素坯11的超导陶瓷材料的第一内连接模块13上面形成，在这种情况下，绝缘材料模块19可以是绝缘模块16的一部分，而不必把它们分别印刷。据此，所有的印刷层都可以在一块素坯的一面上形成，并且这些素坯的压实以及压片的烧结可按如前描述的方法进行。
上面描述的多层衬底可以在坚实的或烧成的陶瓷基底，象氧化铝板30上形成，见图7，在这种情况下，不仅仅金模块23、超导陶瓷材料模块22和绝缘材料24、并且代替素坯21的绝缘层21′都可由厚膜形成方法，如屏蔽印刷法来制备。绝缘材料层21′的厚度一般要大于80μm，最好是100μm到150μm，如120μm。
例3
除了在超导陶瓷材料涂料的准备中，用铜的金属粉末颗粒代替CuO的粉末颗粒，以及超导陶瓷材料形成是在素坯压片的烧成平台上完成以外，其余的与例2相同。
摩尔比为0.6∶0.2∶1的BaCo3，Y2O3和Cu颗粒粉末与粘合剂，萜品醇和丁酮混合起来并搅拌10小时，既成涂料混合物，接下来，再经过30次的滚磨。这样，可得到具有大约2000泊左右的涂料。
这种涂料用于形成超导陶瓷材料模块。形成素坯层压制件的工艺同例2。
层压制件的烧结是在空气、氧或氧与惰性气体的混合体中进行，温度大约950℃，时间12小时。层压制件的退火在850℃的氧气氛中进行，时间为60分钟。烧结以后得到了多层衬底，并且利用四极探针方法测量了其上超导材料模块的电阻，其结果与图1相似，在液氮温度（77K）时电阻下降到零。
例4
除了通孔是由超导陶瓷材料的生成球穿透素坯形成外，其余的工艺与例1的相同。
超导陶瓷材料球按如下方法制备。例如，参照图8，由摩尔比为0.6∶0.2∶1的BaCO3，Y2O3和CuO组成的混合物，在坩埚31中被加热器32加热熔融。熔融陶瓷材料33顺喷嘴34流下。高压气流36经过喷射口37作用在熔融陶瓷材料束流35上，这样熔融陶瓷材料被粉化，冷却以后形成陶瓷材料粉末颗粒38。高压气体可以是氮气（N2），氩气（A2）或空气，其压力为了到5千克/厘米2。据此，利用粉化过程可得到颗粒度为20μm到500μm的超导陶瓷材料球状颗粒。
超导陶瓷材料球体的穿透按如下方式进行，陶瓷材料素坯41放置在具有凹槽43（通孔在此形成）的平板42上。具有锥形孔45（通孔在此形成）的另一块平板44被放置在素坯41上，这样44板上的锥形孔正好处于基板42的凹槽43之上，超导陶瓷材料球46插入到锥形孔45中。带有凸出部48的模具板47放置在具有孔的另一板44上，这样凸出部48正好对应孔45。然后对基板42、素坯41、板44和模具47的组合件进行热压，这样球46穿透了素坯41，就是说，具有由超导陶瓷材料球46形成的穿透孔的素坯41得到了。这一过程的描述在日本已审查专利公报（Kokokn）第58-32797号上，它的叙述一同包括在参考文献中。
利用这种球穿透法，精确的穿孔和孔的填充可同步完成。
超导陶瓷材料球可以是设烧结的超导陶瓷材料球。比如，在例1中所描述的超导陶瓷涂料，利用浇铸可成形为球状体，在此期间，热固化树脂被利用来作为涂料的粘合剂。
例5
在包封超导陶瓷材料模块的金属中加入接合剂，象钛或硅接合剂，有利于改善金属和素坯，特别是象在例2中所见到的多层衬底中的玻璃陶瓷素坯，以及超导陶瓷材料模块的附着力。
例6
在以上例子中，多层衬底被制备出来，其上可安放IC′s，〔S〕′s，V〔S〕′s，约瑟夫森元件等，如图10所示。图中51标记多层衬底，52标记超导陶瓷模块，53标记绝缘层，54标记芯片或元件，如IC′S等。

Claims (34)

1、多层衬底，它包括：
层压在多层衬底上的，具有通孔的多重绝缘层；
在两绝缘层之间的超导陶瓷材料的内连接层；和
填满在上述绝缘层孔中的超导陶瓷材料通孔，此孔把上述内连接层电学上联接在一起。
2、权利要求1中的多层衬底，其中的超导陶瓷材料是一种氧化陶瓷材料，一般分子式为XaY1-aZOb或（X1-aYa）2ZOb，这里O＜a＜1;3 b＜4;X至少是Ba，Ca，Sr和Mg中的一个元素，Y至少是Sc，Y，La，Ce，Pr，Nd，Pm，Sm，Eu，Gd，Tb，Dy，Ho，Er，Tm，Yb和Lu中的一个元素。Z至少是Cu，Ag，Au中的一个元素。
3、权利要求1中的多层衬底，其中的陶瓷超导体是｛（MⅡO）x（MⅢ 2O3）1x｝y（CuO）2（O）δ，这里M代表Ba，Sr，Ca和Mg中的至少一个元素;MⅡ代表Y，Sc，La，Ce，Pr，Nd，Sm，Eu，Gd，Tb，Dy，Ho，Er，Tm，和Lu中的至少一个元素;0.5 X 0.9;1 Y 2;1 Z 2;δ代表氧含量与标准氧化学当量的偏离量;氧化物超导材料在氮沸点温度以上呈现出超导电性。
4、权利要求1中的多层衬底，其中陶瓷超导体为YBa2Cu3O7。
5、权利要求1中的多层衬底，其中陶瓷超导体是超导氧化物Bi-Sr-Ca-Cu-O和TI-Bi-Si-Ca-Cu-O系列中的一个。
6、权利要求1中的多层衬底，它还包括包封陶瓷超导体内连接层的金属层，金属层的金属可选用金、银、铂或其合金。
7、多层衬底，包括：
层压在多层衬底上的，具有通孔的玻璃陶瓷材料的多重绝缘层;
在上述两绝缘层之间的超导陶瓷材料的内连接层;
填满在上述绝缘层孔中的超导陶瓷材料通孔，此孔把上述内连接层电学上联接在一起;
包封上述内连接层和上述通孔的金属层把内连接层和通孔中的超导陶瓷材料与绝缘层隔离开，金属层中的金属可选用金、银、铂或其合金。
8、权利要求7中的多层衬底，其中玻璃陶瓷材料包含20%到50%重量百分比的氧化铝，10%到60%重量百分比的石英玻璃，20%到40%重量百分比的玻璃或结晶化玻璃，该玻璃陶瓷材料在低于1000℃的温度下即可烧成。
9、权利要求7中的多层衬底，其中超导陶瓷材料是氧化陶瓷材料，分子式为XaY1-aZOb或（X1-aYa）2ZOb，这里0＜a＜1;3 b 4;X至少是Ba，Ca，Sr和Mg中的一个元素;Y至少是Sc，Y，La，Ce，Pr，Ud，Pm，Sm，Eu，Gd，Tb，Dy，Ho，Er，Tm，Yb和Lu中的一个元素;Z至少是Cu，Ag和Au中的一个元素。
10、权利要求7中的多层衬底，其中用于包封的金属层厚为5至10μm。
11、权利要求7中的多层衬底，其中内连接层厚度为20μm。
12、权利要求11中的多层衬底，其中内连接层厚度为20到40μm。
13、权利要求7中的多层衬底，其中金属层还包括钛（Ti）或硅（Si）接合剂。
14、多层衬底制备方法，包括如下步骤：
准备绝缘材料素坯;
在每一素坯上成形超导陶瓷材料模块;
制作穿过素坯的超导陶瓷材料通孔;
具有内连接模块和通孔的素坯层叠在一起并压制成形;和
烧结层压制件，这样含有绝缘材料层，超导陶瓷材料内接层和超导陶瓷材料通孔的多层衬底就制得了。
15、制备多层衬底的方法，包括如下步骤：
准备绝缘材料素坯，使之具有第一和第二主表面以及穿过此素坯的孔;
在每一素坯的第一和第二主表面上形成金属涂料模块，金属涂料覆盖住上述素坯通孔的内表面，金属涂料中的金属可以是金、银、铂或其合金，
在金属涂料模块上以及金属涂料内制成超导陶瓷材料的内连接模块，超导陶瓷材料的涂料填满在上述的通孔中;
将具有金属涂料和超导陶瓷材料涂料的素坯层叠起来压紧，以使超导陶瓷材料的内连接模块由金属涂料包封起来并与素坯隔离;
烧结该层压制件，由此包含有绝缘层和由金属涂料包封的超导陶瓷材料内连接模块的多层衬底就得到了。
16、制备多层衬底的方法，包括如下步骤：
准备绝缘材料素坯，使之具有第一和第二主表面以及穿过此素坯的孔;
在每一素坯的第一主表面上形成金属涂料模块，金属涂料中的金属可以是金、银、铂和其一种它们的合金;
在每一素坯的第二主表面上涂上金属涂料形成第二个模块;
在素坯透穿孔的内表面上涂上一层由金属涂料;
在每一素坯的金属涂料模块上以及金属涂料内制成超导陶瓷材料的内连接模块;
用超导陶瓷材料涂料填满素坯的透穿孔;
将素坯层层叠压紧，以使金属涂料把超导金属陶瓷材料的内连接模块包封起来，并用金属涂料使之与素坯隔离，和
烧结该层压制件，由此包含有绝缘层和由金属涂料包封的超导陶瓷材料内连接模块的多层衬底就得到了。
17、制备多层衬底方法，包括如下步骤：
准备绝缘层素坯，使之具有主表面和穿过此素坯的孔;
在每一素坯的主表面上成形金属涂料的第一模块，此金属涂料中的金属可以是金、银、铂或其合金;
在素坯的通孔的内表面上涂上一层金属涂料;
在每一素坯的第一金属涂料模块上以及金属涂料内制成超导陶瓷材料涂料的内连接模块;
用超导陶瓷材料填满素坯的通孔;
在内连接模块上成形金属涂料的第二模块，这金属涂料的第二模块对应于金属涂料的第一模块，以便用金属涂料包封超导陶瓷材料的内连接模块。
将具有由金属涂料包封的超导陶瓷材料内连接模块的素坯层叠压紧;
烧结该层压制件，因此含有绝缘层和由金属包封的超导陶瓷材料内连接模块的多层衬底就得到了。
18、制备多层衬底的方法，包括如下步骤：
准备绝缘陶瓷基底;
在绝缘陶瓷基底上面成形金属涂料的第一模块，金属涂料中的金层可以是金、银、铂和其合金;
在金属涂料的第一模块上以及金属涂料内制成超导陶瓷材料涂料的第一内连接模块;
在超导陶瓷材料涂料的第一内连接模块上成形金属涂料的第二模块以便用金属涂料包封超导陶瓷材料的第一内连接模块;
在绝缘陶瓷基底和金属涂料的第二模块上成形绝缘材料的第二模块以便用金属涂料包封超导陶瓷材料的第一内连接模块;
在绝缘陶瓷基底和金属涂料的第二模块上成形绝缘材料涂料的第一层并使其上具有一透穿孔，穿通绝缘材料涂料的第一层;
在绝缘材料的第一层上面成形金属涂料的第三模块;
用金属涂料覆盖绝缘材料第一层的透穿孔的内表面;
在金属涂料的第三模块上以及金属涂料内制成超导陶瓷材料的第二内连接模块;
在超导陶瓷材料的第二内连接模块上成形金属涂料的第四模块，以便用金属涂料包封超导陶瓷材料涂料的第二内连接模块;
重复上述从绝缘材料涂料的第一层成形到金属涂料的第四层成形的步骤，直到所需要的层数为至;和
烧结包括绝缘陶瓷基底的层压制件，由此含有绝缘层和由金属包封的超导陶瓷材料内连接模块的多层衬底就得到了。
19、权利要求15，16，17的方法，还包括一绝缘材料模块在素坯上形成的步骤，这一绝缘材料模块是金属涂料模块的补充并且其厚度是超导陶瓷材料内连接模块和金属封装模块厚度的和。
20、权利要求15，16，17或18的方法，其中超导陶瓷材料是氧化物陶瓷材料，由一般分子式X Y1ZO或（X1Y）ZO表示，这里0＜a＜1;3 b＜4;X至少是Ba，Ca，Sr和Ma中的一个元素;Y至少是Sc，Y，La，Ce，Pr，Nd，Pm，Sm，Eu，Gd，Tb，Dy、Ho，Er，Tm，Yb和Lu中的一个元素;Z至少是Cu，Ag和Au中的一个元素。
21、权利要求20的工艺，其中超导陶瓷材料涂料包含超导陶瓷材料的粉末颗粒。
22、权利要求20的方法，其中超导陶瓷材料包括元素X，Y和Z的氧化物粉末颗粒，X，Y和Z元素的摩尔比为a∶（1-a）∶1。
23、权利要求20的方法，其中超导陶瓷材料包含元素X和Y的氧化物粉末颗粒以及金属Cu的粉末颗粒，X、Y和Cu的摩尔比为a∶（1-a）∶1。
24、权利要求15，16，17或18的方法，其中绝缘材料是玻璃陶瓷材料。
25、权利要求24的方法，其中玻璃陶瓷材料包含20%到50%重量比的氧化铝，10%到60%重量比的石英玻璃和20%到40重量比的玻璃或结晶玻璃，它能在低于1000℃温度下烧成。
26、权利要求15，16，17或18的方法，其中金属涂料包含钛（Ti）或硅（Si）接合剂。
27、权利要求15，16，17或18的方法，其中层压制件的烧结是在含氧量大于5%的气氛中进行的。
28、权利要求27的方法，其中层压制件的烧结是在800℃到1000℃温区内进行的。
29、权利要求15，16，17或18的方法，其中超导陶瓷材料的涂料包含超导陶瓷粉末颗粒，有机粘合剂和不易挥发溶剂。
30、用于制备超导陶瓷薄膜的涂料，包括超导陶瓷材料粉末颗粒，有机粘合剂和溶剂。
31、用于制备超导陶瓷膜的涂料，包括：通过烧结而形成超导陶瓷材料的配料粉末颗粒，有机粘合剂和溶剂。
32、权利要求30或31的涂料，其中超导陶瓷材料是氧化物陶瓷材料，一般分子式为：XaY1-aZOb或（X1-aYa）2ZOb，这里0＜a＜1;3 b＜4;X至少是Ba，Ca，Sr和Mg中的一个元素，Y至少是Sc，Y，La，Ce，Pr，Nd，Pm，Sm，Eu，Gd，Tb，Dy，Ho，Er，Tm，Yb和Lu中的一个元素;Z至少是Cu，Ag和Au中的一个元素。
33、权利要求30或31的涂料，其中有机涂料可从如下一组材料中选择，Z基纤维素，聚乙烯丁醇，甲基纤维素和丙烯酸基聚合物。
34、权利要求30或31的涂料，其中超导陶瓷材料是超导氧化物Bi-Sr-Ca-Cu-O和Tl-Bi-Sr-Ca-Cu-O系列的一种。
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