CN1149667C - 高热导率氮化硅电路衬底和使用它的半导体器件 - Google Patents

高热导率氮化硅电路衬底和使用它的半导体器件 Download PDF

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CN1149667C
CN1149667C CNB961211156A CN96121115A CN1149667C CN 1149667 C CN1149667 C CN 1149667C CN B961211156 A CNB961211156 A CN B961211156A CN 96121115 A CN96121115 A CN 96121115A CN 1149667 C CN1149667 C CN 1149667C
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silicon nitride
ceramic plate
nitride ceramic
intermediate layer
substrate
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CN1151612A (zh
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��Ұ���
角野裕康
堀口昭宏
加曾利光男
上野文雄
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Toshiba Corp
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Abstract

本发明公开了一种高热导率氮化硅电路衬底，它包括25℃时热导率为60W/m.K以上的氮化硅陶瓷板，和通过中间层与氮化硅陶瓷板连接的金属电路板。中间层包含氧和选自由Ti、Zr、Hf、Nb和Al组成的组中的至少一种元素。及用该衬底的半导体器件。

Description

高热导率氮化硅电路衬底 和使用它的半导体器件
本发明涉及氮化硅电路衬底和使用它的半导体器件，特别涉及其机械强度和抗热循环性提高了的并具有优异辐射特性的高热导率氮化硅电路衬底，和使用它的半导体器件。
近年来，陶瓷板可作为一种电路衬底构件。日本临时特许公开135771/1994号报道了一种主要包含氮化硅的陶瓷板，它不仅具有高的机械强度和耐热性，还有高热导率。
现有技术中，直接连接法，不用诸如腊材料的粘结材料而将陶瓷板连接到金属电路板。该方法是，用加热法使金属电路板中包含的组分或金属电路板的组分和陶瓷板产生低共熔化合物，用低共熔化合物作粘结剂使其实现连接。
该连接法对氧化物陶瓷如氧化铝是有效的，但对氮化物陶瓷无效。因为，低共熔液相的浸润性极低，因而对金属电路板的连接强度不够。本发明人经研究还发现，在氮化物陶瓷中，就氮化铝(AlN)而言，当陶瓷板在含氧气氛如空气中经过热处理，在其表面上形成对低共熔液相有良好浸润性的氧化物层(Al2O3)，但该方法对氮化硅陶瓷板无效。
因而，用常规的直接连接法连接氮化硅陶瓷板和金属电路板时，连接强度降低。而且，当半导体元件在连接部分进行重复热循环时，连接部分附近区域内的陶瓷板上产生破裂，使电路板的抗热循环能力低。
为克服现有技术中存在的上述缺陷提出本发明。本发明的目的是，提供一种高热导率氮化硅电路衬底，它有更高的热导率，更优异的辐射性能、除具有烧结氮化硅陶瓷电路板固有的高强度特性外，其耐热循环能力也明显改善，还提供用所述氮化硅衬底的半导体器件，使其热循环可靠性得到改善。
本发明人发现，通过包含选自钛、锆、铪、铌和铝中至少一种元素和氧的中间层，将金属电路板连接到热导率在25℃为60W/m.K以上的氮化硅陶瓷板上，使电路衬底和半导体器件的机械强度、韧性值，耐热循环能力和辐射特均能令人满意。
按本发明的高热导率氮化硅电路衬底是，在除具有氮化硅烧结体固有的高强度和高韧度特性外还具有显著提高了的热导率的高热导率氮化硅陶瓷板的表面上，形成包含选自Ti、Zr、Hf、Nb和Al中至少一种元素和氧的中间层，并半金属电路板直接连接到中间层，而连接成一个整体状态构成的。因而，在装配步骤中，夹持电路衬底不会发生碎裂，能以高生产率成批生产用该电路衬底的半导体器件。
由于氮化硅衬底的韧性值高，热循环中衬底上极少出现碎裂，因而使半导体器件的耐热循环能力明显改善，具有优异的使用寿命和可靠性。而且氮化硅本身的机械强度优异，因而，当要求机械强度特性恒定时，与其它陶瓷衬底相比，本发明衬底可做得更薄。由于能减小衬底厚度，耐热性可做得更小。即使衬底比常规衬底薄，也能满足要求的机械特性。因而，能实现电路衬底的高密度封装，使半导体器件的尺寸减小。
图1是本发明的高热导率氮化硅电路衬底的平面图；
图2是图1所示的按本发明的高热导率氮化硅电路衬底沿图1中X-X线切开的截面图；
图3是用按本发明的高热导率氮化硅电路衬底的半导体器件的结构图；
图4是用按本发明的高热导率氮化硅电路衬底的另一半导体器件的结构图。
首先说明按本发明的氮化硅陶瓷板。
按本发明的氮化硅陶瓷板包含作为基体的氮化硅，若需要，还包含例如，诸如稀土元素的助烧剂。就优选实施例而言，氮化硅陶瓷板含的稀土元素的量按其氧化物计算为1.0-12.5wt％，和作为阳离子杂质元素的总量为0.3wt％的锂、钠、钾、铁、钙、镁、锶、钡、锰和硼。
按本发明的氮化硅陶瓷板结构上包括氮化硅颗粒，晶界相和最好是1.5vol％以下的孔率。晶界相中存在的结晶化合物相以总晶界相为基是20vol％以上，更好是50vol％以上。
按本发明的氮化硅陶瓷板的物理特性是：在25℃的热导率为60W/m.K以上，最好是80W/m.K以上，室温的3点弯曲强度是60kgf/mm2以上。最好是80kgf/mm2。
用以下方法制备用于本发明的高热导率氮化硅陶瓷板。预先确定必需的添加剂如助烧剂和有机粘结剂的数量，并将其加到有细颗粒的和杂质含量少的氮化硅粉中，搅拌混合物，制备起始混合物，然后，用诸如通用的金属模压法或刮板法等薄片形成法，获得有预定形状的成型品。在预定温度，例如最高温度为600-800℃，在无氧气氛中对成形制品脱脂，将获得的脱脂后产品在预定温度，经预定时间，在诸如氮气和氩气的惰性气体气氛中加压烧结，然后按预定的冷却速度逐渐冷却，获得致密烧结体。如果需要，将烧结体经过研磨工艺等，可获得有预定形状的高热导率的氮化硅陶瓷板。
作为按本发明的高热导率氮化硅陶瓷板的主要起始材料的氮化硅粉要考虑烧结性能、强度和热导率，细氮化硅粉中氧含量为1.7wt％以下，最好是0.5-1.5wt％，Li、Na、K、Fe、Mg、Ca、Sr、Ba、Mn、B等杂质阳离子元素的含量是0.3wt％以下，最好是0.2wt％以下，具有优异烧结性能的α相氮化硅的量为90wt％以上，最好是93wt％以上，平均颗粒尺寸是0.8μm以下，最好是0.4-0.6μm。
用平均颗粒大小为0.8μm以下的细起始粉，少量助烧剂，能获得孔率为1.5vol％以下的致密烧结体。用较低热导率的元素Li、Na、K、Fe、Mg、Ca、Sr、Ba、Mn和B作杂质阳离子元素，以确保热导率在60W/m.K以上，必须使上述杂质阳离子元素的总含量在0.3wt％以下。用含烧结性能比β相氮化硅好的α相氮化的氮化硅起始粉的量为90wt％以上，能制成高密度和高热导率的氮化硅陶瓷板。
添加到氮化硅起始粉中作为助烧剂的稀土元素可以是Y、La、Sc、Pr、Ce、Nd、Dy、Ho、Gd等的氧化物，或经热处理后能成为这些氧化物的化合物，例如，碳酸盐，硝酸盐，草酸盐和醇盐。若需要可将这些氧化物和化合物中两种以上的氧化物或化合物组合添加，但特别优选氧化钇(Y2O3)。烧结步骤中上述助烧剂与氮化硅起始粉反应生成液相，并加速烧结。
欲添加的上述助烧剂的用量以起始粉量为基按氧化物计算规定为1.0至12.5wt％。若添加的助烧剂量少于1.0wt％，加速烧结作用不充分，但是，若添加量超过12.5wt％，则会产生过量的晶界相，造成低的热导率和低的机械强度。添加量的较好范围是3.0至6.0wt％。
而且添加氧化铝(Al2O3)和氮化铝中至少一种作为另一种成分时，氧化铝和/或氮化铝与上述稀土元素反应生成液相，因而能获得加速烧结作用，特别是在加压下烧结时，有明显作用。若要添加的这些成分的总量小于0.1wt％，则密度不够，若超过2.0wt％，会产生过量的晶界相，或在氮化硅中出现部分铝原子固熔体，使热导率降低。因而，要求添加量规定在0.1至2.0wt％范围内，最好是在0.2至1.5wt％范围内。
关于其它成分，可添加Ti、Zr、Hf、V、No、Ta、Cr、Mo、和W的氧化物、碳化物、氮化物、硅化物和硼化物等等。这些化合物的作用是增强晶格结构中的弥散并提高氮化硅衬底的机械强度。若上述化合物的添加量小于0.2wt％，提高强度的作用小，若添加量超过3.0wt％，则使热导率降低和介质击穿强度下降。因而，要求规定添加量在0.2至3.0wt％，最了在0.3至2.0wt％。
而且上述如Ti、Zr、和Hf的化合物还起光屏材料的作用，它使氮化硅陶瓷板变色并使其变暗。为此，当氮化硅陶瓷板用作其中安装有容易由光引起误动作的集成电路等的电路板时，特别要求添加上述化合物。
为好使氮化硅陶瓷板的孔率在1.5vol％以下，氮化硅烧结体中形成的晶界相包含20vol％以上的晶相，必须将氮化硅制成品在1800至2000℃在加压条件下烧结0.5至10小时，烧结完成后将冷却速度调节并控制在100℃/小时以下，最好是50℃/小时以下。当规定烧结温度低于1800℃时，烧结体密度不足，使机械强度和热导率下降。另一方面，若烧结温度超过2000°，氮化硅的分解和气化变得非常有害。
烧结后的冷却速度对于晶化晶界相和获得高机械强度和高热导率来说是重要的因素，当进行冷却速度超过100℃/小时的快速冷却时，烧结体内部的晶界相中包含的无定型(非晶相)的生成速率变大，会降低机械强度和热导率。
在预定烧结温度(1800℃至2000℃)至由上述助烧剂反应生成的液相凝固的温度范围内，严格控制上述冷却速度。例如，在用上述助烧剂的情况下液相凝固温度是约1500℃至1600℃。在烧结温度至液相凝固温度的温度范围内，将冷却速度控制到100℃/小时以下，最好是50℃/小时以下，晶界相变成晶相的比例是20vol％以上，最好是50vol％以上，因而能获得有优异机械强度和热导率的氮化硅陶瓷板。
随后，说明按本发明的包含氧和选自Ti、Zr、Hf、Nb和Al中至少一种元素的中间层。
含氧和选自Ti、Zr、Hf、Nb和Al中至少一种元素的中间层可以是诸如铝酸盐和硅酸盐的上述元素的氧化物和化合物，例如，含铝的中间层可以是诸如Al2O3、莫来石(Al2O3-SiO2)，稀土元素的铝酸盐和SIALON等的化合物。而且，含这些金属元素的非晶层如玻璃等也是合适的。中间层中含的元素和氧改善金属电路板的低共熔液相的浸润性。与此同时，生成含中间层中所包含的金属元素的化合物和金属电路板构成元素氧，使金属电路板与中间层牢固地连接，而且，中间层与氮化硅陶瓷板也能牢固连接。还发现，特别是金属电路板主要含铝和中间层包含铝时，金属电路板的铝与中间层中含的铝相互扩散，使其牢固连接。
最好规定中间层的厚度在0.5-10μm范围内。若厚度在上述范围内，则能更好地改善上述低共熔液相的浸润性，这对中间层的耐热性几乎无损害，并能容易地减小中间层与氮化硅陶瓷板之间的热膨胀系数之差。厚度范围规定在1至5μm最好。
烧结之后，用各种方法在氮化硅陶瓷板表面上形成上述中间层。所述方法可以是，用溶胶-凝胶法，浸渍法，或旋涂法形成变成初始物的均匀膜，然后对该膜热处理，制成所要求的化合物的中间层，或用CVD法PVD法等形成直接变成中间层的化合物层。在玻璃中包含上述元素的情况下，将玻璃细粉制成浆料，将浆料均匀涂在氮化硅陶瓷板上，然后加热使其熔化。而且，为了提高中间层与氮化硅陶瓷层的连接强度，可在中间层形成后进行热处理。根据中间层的特性要求选择热处理的温度和气氛等条件。温度最好在800℃以上，气氛最好是空气。
而且，制备氮化硅陶瓷板时，可预先采用形成中间层的方式。即，在制备氮化硅陶瓷板的步骤中有制备脱脂产品的阶段，将上述脱脂产品浸渍包含钛、锆、铪、铌或铝的醇盐，使过量上述金属只存在于脱脂产品表面附近，烧结脱脂产品，制成在其表面上存在过量上述金属的氮化硅陶瓷板。随后，在含氧气氛中对氮化硅陶瓷表面进行热处理，形成所要求的中间层，并使金属电路板连接到中间层。
例如，用含铝的醇盐溶液进行上述处理时，在氮化硅陶瓷板表面上形成会变成中间层的诸如Al2O3，或SiO2-Al2O3化合物SIALON等的氧化物表面层。
以下说明按本发明的金属电路板。
可以是金属电路板的金属没有特别限定，只要是Cu、Al、Fe、Ni、Cr、Ag或Co的简单物质，含氧的上述金属、或上述金属的合金等，它能产生低共熔液相并能连接。但是，从电导率和价格上考虑，选用Cu、Al、Ni及其合金(它们全都可以含一定量的氧)。
例如，金属电路板是铜的情况下，用下述方法连接金属电路板。即，在高热导率氮化硅陶瓷板的预定位置上形成有规定厚度的含氧和选自Ti、Zr、Hf、Nb、和Al中至少一种元素的中间层，与含氧铜电路板接触，在铜或氧化铜(Cu2O)的低共熔(1065℃)温度以上的温度加热铜电路板并持续一定时间，若需要，可加负荷，以产生低共熔液相，并用液相作连接剂，将铜电路板连接到高热导率氮化硅陶瓷板。也可用其它类金属电路板，但在那种情况下，必须设定能产生低共熔液相的热处理温度。
按本发明的半导体器件是其中的半导体元件安装在上述高热导率氮化硅电路衬底上的器件。就使用高热导率的氮化硅电路衬底的特别典型的例子而言，可以是称作大功率组件的半导体器件，其中安装有高输出半导体元件，例如，双极性晶体管IGBT或GTR。这些半导体器件主要用于控制各种电机，大电功率开关等。随着半导体器件的驱动和停止，对半导体元件进行加热和冷却的热循环，由于上述氮化硅电路衬底具有高强度，高热导率和高可靠性，因而该器件能足以适应这种热循环。而且，它们能用于安装半导体元件的封装。
实施例
下面参照实施例详细说明本发明。用实施例说明是为了便于理解本发明，但实施例不是对发明的特别限制。
例1
氮化硅起始粉包含1.3wt％的氧，0.15wt％的杂质阳离子元素，97％的α相型氮化硅，平均颗粒大小为0.55μm，作为助烧剂的平均颗粒大小为0.7μm的氧化钇(Y2O3)粉和平均颗粒大小为0.6μm的氧化铝(Al2O3)粉，其添加量分别是总重量的5wt％和1.5wt％。把混合物在乙醇中研磨24小时，然后干燥，制成起始混合粉材料，给所获得的起始混合粉材料中加有机粘接剂，并搅拌混合物，然后，在1吨/厘米2的压力下模压混合粉，制成大小为80×50×1mm3的模压制品。随后，在最高温度为700℃的氮气中对获得的模压制品脱脂，将制成的膜脂产品在7.5个大气压，在1900℃在氮气中烧结6小时，然后按100℃/小时的冷却速度冷却到1500℃，然后进行炉内冷却，获得致密的氮化硅烧结体。然后，研磨烧结体，获得厚度为0.6mm的氮化硅陶瓷板。
然后，用以下方法制备连接用中间层。首先，将丁醇锆(Zr(OBu)4)溶解于溶剂丁醇中，用溶剂稀释水，使溶液中不形成沉淀，然后滴加于溶液中，使其部分水解。然后，将用溶剂稀释过的浓盐酸滴加到溶液中。搅拌并回馏混合物，制成涂覆溶液。将上述氮化硅陶瓷板浸入涂覆溶液中，按1.5cm/秒的速度提起，并干燥。浸渍并干燥的步骤重复10次后，氮化硅陶瓷板在1200℃在空气中保持1小时，在氮化硅陶瓷板上形成厚0.8μm的氧化锆(ZrO2)层。
随后，在氮化硅陶瓷板的两边形成中间层，与包括厚度为0.3mm的韧铜的铜电路板保持接触状态，将板放入钟罩型加热炉中，在1073℃最高温度在氮气氛中保持1分钟，使铜电路板连接到氮化硅陶瓷板上，由此获得图1所示的高热导率氮化硅电路衬底。图1中，2是氮化硅陶瓷板，4是金属(Cu)电路板。
测试所获得的氮化硅电路衬底的热导率时，热导率是80W/m.K，孔率是0.18vol％，用粉末X-射线衍射法测得的晶界相中的晶相比是33Vol％。
为了测试获得的电路衬底的强度特性和韧性，测试3点弯曲强度和最大挠度。在上述电路衬底的中心部分加负荷，在支撑跨度为50mm支撑电路衬底的状态下测试最大挠度，并测试至电路衬度断裂时的最大挠度限，结果所测得的3点弯曲强度是64kg/mm2，最大挠度是1.2mm。
为了评估铜电路板与氮化硅陶瓷板连接部分的连接强度，测试剥离强度。将厚度为0.3mm，宽度为3mm的韧铜板连接到其上形成有中间层的氮化硅陶瓷板上，用与上述方法相同的方法，将韧铜板的端部在相对于衬底90°的方向向上剥离，用Instron测试仪测试剥离强度。那时的十字头速度是50mm/分钟。结果，剥离强度是7.9kgf/cm，连接强度足够。
在耐热循环试验中，电路衬度从-45℃加热至室温，随后将其从室温加热到+125℃，然后将其冷却，经室温至-45℃，以此定为一个周期，对电路衬底重复该周期，该周期的循环次数是至衬底部分出现碎裂等现象时评估的，甚至在循环到第1000次时也没在衬底部分出现碎裂。
高热导率氮化硅电路衬底上安装多个半导体元件，制成图3所示半导体器件。图3中，6是半导体器件，7是氮化硅陶瓷板，8是金属(Cu)电路板，9是金属电路板(背面Cu板)，10是半导体元件，11是连接线，12是引线端，13是焊料，14是引线端。使电通过半导体器件，测试瞬时耐热性，所述器件具有与用常规氮化铝衬度的半导体器件同样优异的辐射性。而且，无论是在氮化硅衬底内部或氮化硅陶瓷板与铜板的连接部分均未发现碎裂产生。因而可以证明氮化硅衬底有优异和耐久性和可靠性。
例2
用例1相同的方法进行烧结工艺后，不控制冷却工艺，烧结体在炉内冷却至室温，获得热导率为36W/m.K的致密氮化硅烧结体。那时的平均冷却速度是500℃/小时。然后，用与例1相同的方法形成ZrO2中间层，用与例1相同的方法连接铜层，制成电路衬底。所获得的氮化硅电路衬底的3点弯曲强度是72kgf/mm2。最大挠度是1.1mm，耐热循环测试中，甚至经1000次循环在衬度上也没产生破裂。
例3
首先用与例1相同的方法获得厚0.6mm的氮化硅陶瓷板。
随后，用以下方法制备用于连接的中间层。首先，将丁醇铝溶解于溶剂2-丁醇中，用溶剂稀释水，使溶液中不生成沉淀，然后滴加溶液使其部分水解。此后，用溶剂稀释浓盐酸，然后滴加到溶液中。搅拌并回馏混合物，制成涂覆溶液。将上述氮化硅陶瓷板浸入涂覆溶液中，按1.5cm/秒的速度提起并干燥。重复浸入和干燥步骤10次后，氮化硅陶瓷板在1200℃，在氮气中保持1小时，在氮化硅陶瓷板上形成厚1.2μm的氧化铝(Al2O3)层。
随后，在氮化硅陶瓷板的两边形成中间层，与含韧铜的厚0.3mm的铜电路板接触，将该板放入钟型加热炉内，在最高温度为1075℃在氮气气氛中加热1分钟，使铜电路板与氮化硅陶瓷板连接，由此获得图1所示高热导率氮化硅电路衬底。
测试获得的氮化硅衬底的热导率时，热导率为76W/m.K孔率为0.2vol％，用粉末X-射线衍射法测得的晶界相中的结晶相比为30vol％。
为了测试获得的电路衬底的强度特性和韧性，按实施例1的方法测试3点弯曲强度和最大挠度。结果，3点弯曲强度是68k.gf/mm2，最大挠度是1.2mm。按实施例1的方法测试剥离温度的结果是7.4kgf/cm，证明有足够的密度和强度。并按实施例1的方法进行耐热循环测试，在第1000次循环时在衬底部分未发生破裂。
在高热导率氮化硅电路衬底上安装多个半导体元件，制备图3所示半导体器件。使电通过半导体器件测试瞬时耐热性，所述器件有用常规氮化铝衬底的半导体器件同样优异的辐射性能。而且，无论是在氮化硅衬底内部还是在氮化硅陶瓷板与铜板的连接处均未发现破裂等产生。因此证明，半导体器件有优异的耐久性和可靠性。
例4
在例2中获得的氮化硅陶瓷板上，用与例3相同的方法形成Al2O3中间层，用与例3相同的方法连接铜板，制备电路衬底。所获得的氮化硅电路衬底的3点弯曲强度是64kgf/mm2，最大挠度是1.0mm，耐热循环测试中，甚至在循环第1000次时也没在衬底上产生破裂。
例5
用与例1相同的起始氮化硅粉，平均颗粒大小为1.0μm的氧化镝(Dy2O3)粉和平均颗粒大小为0.6μm的氧化铝(Al2O3)粉作助烧剂加入氮化硅起始粉中，其用量分别是总重量的5wt％和0.8wt％。用与例1相同的方法成形和脱脂。然后，在1930℃在氮气中在7个大气压压力下烧结6小时。烧结后，按冷却速度50℃/小时使烧结体冷却至1500℃，然后炉冷至室温，获得致密的氮化硅烧结体。研磨氮化硅烧结体，获得厚度为0.5mm的氮化硅陶瓷板。
所获得的氮化硅陶瓷板的孔率为0.2vol％。晶界相中的结晶相比例为45vol％，热导率高达84W/m.K。
随后，用以下方法制备连接金属电路板用中间层。首先，将四乙氧基钛(Ti(OEt)4)溶解于乙醇溶剂中，并将把水和硝酸(HNO3)加于乙醇获得的混合物滴加到溶液中，回馏生成溶液。用溶剂稀释浓盐酸，然后滴加于溶液中。搅拌并回馏混合物，制备涂覆溶液。把回馏后的溶液加入乙醇中加有预定量水的溶液中，然后再加异丙氧基铝(Al(iso-opr)3)，再对混合物充分回馏。用溶剂稀释浓盐酸，然后滴加于溶液中。搅拌并回馏混合物，制成涂覆溶液。将上述氮化硅陶瓷板浸入涂覆溶液中，按1.0cm/sec速率提起并干燥。重复浸入和干燥步骤15次后，氮化硅陶瓷板在1200℃，在空气中保持1小时，在氮化硅陶瓷板上形成厚1.2μm的铝酸钛(TiAl2O5)层。
随后，在氮化硅陶瓷板的两边上形成铝酸钛中间层，与含韧铜的厚度为0.3mm的铜电路板接触，并将板放入钟罩型加热炉，在最高温度为1075℃在氮气氛中热处理1分钟，使铜电路板连接到氮化硅陶瓷板上。
为测试获得的电路衬底的强度特性和韧性，按与例1相同的方法测试3点弯曲强度和最大挠度。结果，3点弯曲强度是84kgf/mm2，最大挠度是1.3mm。为评估铜电路板与氮化硅陶瓷板的粘接强度而测试剥离强度时，其剥离强度最大值是6.9kgf/cm。
而且，用与例1相同的方法进行耐热循环测试，甚至在第1000次循环时在衬底部分也没发生破裂。
例6
正硅酸乙酯(Si(OEt)4)溶解于乙酸溶剂中，用给乙醇中加水和硝酸(HNO3)获得的混合物滴加到溶液中，并回馏生成的溶液。将回馏后的溶液加于乙醇中溶解有预定量水的溶液中，再加入异丙氧基铝(Al(iso-opr)3，再充分回馏混合物。用溶剂稀释浓盐酸并滴加入溶液。搅拌并回馏混合物，制成涂覆溶液。将例5中获得的氮化硅陶瓷板浸入涂覆溶液中，按1.0cm/sec的速率提出并干燥。浸入并干燥步骤重复15次后，氮化硅陶瓷板在1200℃，在空气中保持小时，在氮化硅陶瓷板上形成厚1.2μm的莫来石膜(3Al2O3-2SiO2)。
随后，在氮化硅陶瓷板的两边上形成中间层，与含韧铜的厚0.3mm的铜电路板接触，将板放入钟罩型加热炉内，在最高温度1075℃，氮气氛中热处理1分钟，使铜电路板连接到氮化硅陶瓷板上。
为测试所获得的电路衬底的强度和韧性，用与例1相同的方法测试3点弯曲强度和最大挠度。结果，3点弯曲强度为84kgf/mm2，最大挠度是1.3mm。为评估铜电路板与氮化硅陶瓷板的粘接强度而测试剥离强度时，其剥离强度最大值为6.9kgf/cm。
而且，用与例1相同的方法进行耐热循环测试，甚至循环到第1000次时，衬底部分也不产生碎裂。
对比例1
用与例1相同的方法制成氮化硅陶瓷板，只是在一个板上不形成中间层，而另一板在1300℃在空气中加热12小时，使其在表面上形成厚2μm的氧化硅(SiO2)层。用与例1相同的方法分别连接铜电路板。并对每个板测试剥离强度，以评估每个板的粘接强度。结果，在氮化硅陶瓷板上没形成中间层，电路板不能连接。另一方面，电路衬底中中间层是SiO2层，剥离强度为2.7kgf/cm的低值，因而，所述衬底不能实用。
对比例2
用与例1相同的方法，只是用厚度为0.6mm，热导率为70W/m.K的氮化铝(AlN)衬底代替例1中的氮化硅陶瓷板，用与例1相同的方法连接铜电路板制备电路衬底。连接铜电路板时，将衬底在氧气氛中热处理而在氮化铝衬底表面上形成的氧化层(Al2O3)用作中间层。尽管所获得的电路衬底的剥离强度是足够大的8.1kgf/cm，3点弯曲强度是30kgf/mm2，最大挠度是0.4mm。在耐热循环试验中，循环到第150次时，产生碎裂。因此，发现与氮化硅电路衬底相比氮化铝电路衬底的机械强度有问题。
例7至14
用与例1相同的方法制备氮化硅陶瓷板。按与例1相同的浸入法，用醇盐溶液在氮化硅陶瓷板表面上，分别形成用于连接的不同化合物中间层。用低共熔液相将Cu、Al或Ni电路板分别连接到中间层表面，制成电路衬底(见表1)。在含Si元素的Al电路板中，连接中的最高温度规定为585℃，在含氧的Ni电路板中，连接中的最高温度规定为1445℃，它高于铜电路板的连接温度。评估电路衬底的剥离强度，进行热循环试验，以考查可靠性，所有电路衬底中，金属电路板牢固地连接到氮化硅陶瓷板上，甚至热循环进行到1000次时，也没产生碎裂等问题。
                                      表1
中间层(厚度) 金属电路板 剥离强度(kgf/cm) 热循环测试(次数)
  例7   HfO2     (2.2μm)   Al     7.4   ＞1,000
  例8   ZrAlO4   (1.3μm)   Cu     8.4   ＞1,000
  例9   Nb2O5   (3.2μm)   Cu     6.3   ＞1,000
  例10   TiO2     (0.8μm)   Ni     8.7   ＞1,000
  例11   Al2O3   (2.2μm)   Al     7.6   ＞1,000
  例12   Y3Al5O12(1.3μm)   Cu     8.4   ＞1,000
  例13   Mullite   (3.0μm)   Cu     6.3   ＞1,000
  例14   Al2O3   (0.8μm)   Ni     7.1   ＞1,000
例15
氮化硅起始粉含1.7wt％的氧和0.13wt％的杂质阳离子元素，含93％的α相氮化硅，其平均颗粒大小为0.6，并分别添加占总重量4wt％和1.2wt％的平均颗粒大小为0.7μm的氧化钬(Ho2O3)粉，和平均颗粒大小为0.5μm的Al2O3粉作助烧剂。随后用与例1相同的方法进行脱脂处理，获得脱脂制品。随后，脱脂产品在1880℃在氮气气氛中在8.1个大气压力下保持8小时使其致密，然后，按50℃/小时的冷却速度冷至1500℃，然后再冷至室温，获得致密的氮化硅烧结体。研磨烧结体，获得厚0.6mm的氮化硅陶瓷板。
然后，用以下方法在氮化硅陶瓷板表面上制备连接金属电路板的中间层。将氮化硅陶瓷板放入溅射设备中，使其与Ti靶相对，用Ar分压为0.1Pa，O2分压为0.2Pa的压力溅射Ti。在氮化硅陶瓷板的两边进行该溅射。结果，在氮化硅陶瓷板表面上获得厚1.5μm的结晶度差的TiO2薄膜。
在其表面上有TiO2薄膜的氮化硅陶瓷板的两边上设置呈接触状态的厚度为0.3mm含韧铜的铜电路板，将板放入钟罩型加热炉内，在最高温度为1075℃，在氮气氛中热处理1分钟，使铜电路板连接到氮化硅陶瓷板上。
获得的氮化硅衬底的孔率为0.2vol％，晶界相中结晶相比率为55vol％，热导率为96W/m.K。测试铜连接于其上的电路衬底的3点弯曲强度和最大挠度量，并对其进行耐热循环试验，测试其剥离强度。结果，3点弯曲强度是75kgf/mm2，最大挠度量是1.1mm，耐热循环试验结果是1000次以上，剥离强度是8.2kgf/cm，因此，所有指标均优，因此该氮化硅电路衬底足以实用。
例16
用与例15相同的方法进行脱脂处理，制成厚0.8mm的氮化硅脱脂产品。此后，将脱脂产品浸入例1中为形成中间层而制备的醇盐溶液中并迅速提出。用与例1相同的方法烧结和冷却产品，获得厚0.6mm的致密氮化硅烧结体。用EPMA检验氮化硅烧结体内部的Zr分布，在烧结体表面附近检到大量Zr，而在烧结体内部只检到少量Zr。当烧结体在1300℃在空气中热处理12小时后，在烧结体表面上形成约2.2μm厚的氧化层。用粉末X-射线衍射法鉴别氧化层的结构相时，发现ZrSiO4。用与例1相同的方法将铜电路板连接到制成板上，制成电路衬底。
获得的氮化硅衬底的孔率是0.2vol％，晶界相中的结晶相比例是47Vol％，热导率是72W/m.K。获得的电路衬底的3点弯曲强度是64kgf/mm2，最大挠度量是1.0mm，耐热循环试验结果是1000次以上，剥离强度是6.9kgf/cm。因此电路衬底的特性优良，氮化硅电路衬底极其实用。
例17
用以下方法制备将金属电路板连接到例15中获得的氮化硅陶瓷板的表面用的中间层。将氮化硅陶瓷板放入溅射设备中，使其对着Al靶放置，用Ar分压为0.1Pa和O2分压为0.2Pa的压力溅射Al。结果，在氮化硅陶瓷板表面上获得厚1.5μm的非晶Al2O3薄膜。
在其表面上有非晶Al2O3薄膜的氮化硅陶瓷板的两边，设置呈接触状态的厚度为0.3mm的含韧铜的铜电路板，将板放入钟罩型加热炉，在最高温度为1075℃，在氮气氛中热处理1分钟，使铜电路板连接到氮化硅陶瓷板上。
获得的氮化硅衬底的孔率是0.2vol％，晶界相中的结晶相比率是55vol％，热导率是96W/m.K。测试铜连接于其上的电路衬底的3点弯曲强度，最大挠度量，并进行耐热循环试验，和剥离强度试验，其结果是，3点弯曲强度是68kgf/mm2，最大挠度量是1.1mm，耐热循环试验结果是1000次以上，剥离强度是9.2kgf/cm。因此所有指标值均优。氮化硅电路衬底极其实用。
例18
用与例15相同的方法进行脱脂处理，制备厚0.8mm的氮化硅脱脂产品。此后，将脱脂产品浸入例3中为形成中间层而制备的醇盐溶液中几秒钟，然后迅速提出。用与例15相同的方法烧结并冷却产品，获得厚0.6mm的致密氮化硅烧结体。用粉末X-射线衍射法鉴别氮化硅烧结体的表面的结构相，发现存在少量氮化硅和大量的SIALON。用EPMA检验氮化硅烧结体内部的铝分布，发现在烧结体表面附近有大量Al，而在烧结体内部只有少量Al。烧结体在1300℃，在空气中热处理12小时后，在烧结体表面上形成厚2.2μm的氧化层。用粉末X-射线衍射法鉴别氧化层的结构相时发现有少量SiO2和大量莫来石。把制成板用作电路衬底，用与例1相同的方法连接铜电路板，制成电路衬底。
获得的氮化硅衬底的孔率是0.2vol％，晶界相中的结晶相比率是47vol％，热导率是72W/m.K。获得的电路衬底的3点弯曲强度是64kgf/mm2，最大挠度量是1.0mm，耐热循环试验结果是1000次以上，剥离强度是6.9kgf/cm。因此，作为电路衬底其性能优良。氮化硅电路衬底极其实用。

Claims (5)

1 高热导率氮化硅电路衬底，它包括25℃时热导率在60W/m.K以上的氮化硅陶瓷板，通过中间层与氮化硅陶瓷板连接的金属电路板，中间层含氧和选自由Ti、Zr、Hf、Nb、Al组成的组中的至少一种元素，
其中，氮化硅陶瓷板含按氧化物计算的含量为1.0到12.5wt％的稀土元素，和Li、Na、K、Fe、Ca、Mg、Sr、Ba、Mn和B为阳离子杂质，杂质总含量是0.3wt％以下。
3 按权利要求1的衬底，其特征是，氮化硅陶瓷板含氮化硅颗粒和晶界相，在晶界相中存在占全部晶界相20vol％以上的结晶化合物相。
4 按权利要求1的衬底，其特征是，中间层厚度是0.5至10μm。
5 按权利要求1的衬底，其特征是，金属电路板包括Cu、Al或Ni。
6  一种半导体器件，其中半导体元件安装在陶瓷电路衬底上，其特征是，陶瓷电路衬底包括在25℃时热导率为60W/m.K以上的氮化硅陶瓷板，和通过中间层与氮化硅陶瓷板连接的金属电路板，中间层含氧和选自由Ti、Zr、Hf、Nb和Al组成的组中的至少一种元素，
其中，氮化硅陶瓷板含按氧化物计算的含量为1.0到12.5wt％的稀土元素，和Li、Na、K、Fe、Ca、Mg、Sr、Ba、Mn和B为阳离子杂质，杂质总含量是0.3wt％以下。
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