CN100509707C - 用于金属或陶瓷的接合剂以及由其接合金属或陶瓷的方法 - Google Patents

用于金属或陶瓷的接合剂以及由其接合金属或陶瓷的方法 Download PDF

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CN100509707C
CN100509707C CNB028188888A CN02818888A CN100509707C CN 100509707 C CN100509707 C CN 100509707C CN B028188888 A CNB028188888 A CN B028188888A CN 02818888 A CN02818888 A CN 02818888A CN 100509707 C CN100509707 C CN 100509707C
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joint compound
metal
powder
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增田次男
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Honda Motor Co Ltd
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Abstract

本发明提供了一种用于金属或陶瓷的接合剂，所述接合剂含有0.25重量%至18.0重量%的镁粉、25重量%至50重量%的分子结构中含有羟基的溶剂以及余量的AlN粉末。使上述接合剂的各组分混合并处于一定的条件之下，这些组分间将发生反应生成大量的反应热。当母材或与之接合的部件是铝合金时，通常形成于其表面上的致密氧化膜会阻碍它们之间的接合，而上述的反应热可使阻碍母材与部件之间接合的这层致密的氧化膜发生热破坏。

Description

用于金属或陶瓷的接合剂以及由其接合金属或陶瓷的方法
技术领域
本发明涉及用于接合金属或陶瓷部件的、基于无机组分的接合剂，更具体而言，本发明涉及通过加热来促进固化的、用于金属或陶瓷部件的接合剂，并涉及采用该接合剂来接合金属或陶瓷部件的方法。
背景技术
已知接合金属或陶瓷部件的方法有焊接(硬焊)或通过有机粘合剂接合的方法。
采用有机粘合剂的接合方法需要昂贵的设备来保持适当的工作环境，因为这种方法采用了如甲苯等有机溶剂。此外，它需要昂贵的设备来处置被污染的有机溶剂。
焊接不会造成任何环境问题及废液的处理问题，但需要在真空炉内将带有焊料的母材及与之接合的部件加热到该焊料的熔化温度(640℃)。暴露在如此高的温度下的母材等会因其内外温差或上下表面的温差而发生热变形。一般通过给母材施加高压来抑制其热变形。这样，焊接法需要采取措施来保护母材等不因加热至高温而发生变形，所以该方法的制造成本高昂。
发明内容
本发明的第一个方面提供了一种用于金属或陶瓷的接合剂，所述接合剂含有0.25重量％～18.0重量％的镁粉和25重量％～50重量％的羟基溶剂，该接合剂组成中的其余部分为AlN粉末。
具有上述组分的接合剂通过其组分间的反应产生大量反应热。此反应热可使存在于母材表面的或与该母材接合的部件表面的任何致密的氧化膜发生热破坏。其中，当母材及与之接合的部件是铝合金时，其表面上存在的致密氧化膜会形成阻碍其接合的隔离层。
获得用来破坏上述氧化膜的热量的方法有将自生热量和外部加热相结合的方法，或仅通过外部加热的方法。与仅通过外部加热的方法相比，将自生热量和外部加热相结合的方法仅需要较少的外部热量。从外部供给的热量越少就可以限制母材及与之接合的部件的温度上升。限制温度上升可以降低母材及与之接合的部件的温度。如果其温度低于当前可能采用的温度，则无需采取特别措施来防止其热变形。即使在可以采取某些措施来防止热变形时，也仅需采用低的夹持压力就足够了。
现有的任何有机粘合剂均可能产生有害气体，但是本发明不产生任何此类气体，因而可以保持良好的环境。
所述羟基溶剂可以是水。
本发明的第二方面提供了一种金属或陶瓷的接合方法，所述方法包括：捏和步骤，其中，为了得到一种接合剂而对镁粉和AlN粉末进行捏和，所述接合剂含有0.25重量％～18.0重量％的镁粉和25重量％～50重量％的羟基溶剂，该接合剂组成的其余部分为AlN粉末；混合步骤，其中，在即将涂布前，向上述捏和后的粉末中混入25重量％～50重量％的羟基溶剂；涂布步骤，其中，用所得到的接合剂涂布金属或陶瓷母材和与之接合的部件这两方中的至少一方；紧贴步骤，其中，采用所述接合剂使所述部件和所述母材紧贴；和加热步骤，其中，将保持彼此紧贴状态的所述母材和所述部件加热到150～500℃，以便促进其接合。
在加入所述羟基溶剂前将上述粉末捏和混匀，这样更容易发生随后的反应。
由于向所述捏和的粉末中加入所述羟基溶剂可引发反应，所以在即将涂布前进行该项混合步骤。
用于使致密的氧化膜发生热破坏的热量来自自生热量和外部加热的结合。于是，加热到150～500℃就足以破坏致密的氧化膜。150～500℃的温度远低于仅采用外部加热时所达到的温度。
附图说明
图1是用本发明的接合方法制造的大电流动力装置的截面图；
图2A～图2C是采用本发明的接合剂接合大电流动力装置的部件的方法示意图；
图3A～图3D是采用不同于图2A～图2C的条件和步骤来接合大电流动力装置的部件的方法示意图；
图4A～图4C是接合发动机气缸与气缸盖的方法示意图；
图5是气缸体的接合作业的准备阶段示意图；
图6是将铝合金片插入气缸内的方法示意图；
图7是图6所示的插入铝合金片的方法的细节示意图；
图8是气缸体的接合作业的加热方法示意图；和
图9是所完成的气缸体的主要部件的透视图。
具体实施方式
首先，将基于如下比例式来说明本发明接合剂的组分的优选范围：
AlN∶Mg∶H2O＝8∶3∶12(系数比)
＝328∶72∶216(重量比)
＝53重量％：12重量％：35重量％
AlN的分子量为41(原子量之和)，乘以8得328。Mg的原子量约为24，乘以3得72。H2O的分子量为18，乘以12得216。
于是，当把8∶3∶12(系数比)换算为重量比时就表示为328∶72∶216。换算为百分数时就是53重量％∶12重量％∶35重量％。换言之，AlN的比例优选53重量％，Mg的比例优选12重量％，H2O的比例优选35重量％。然而，在实际应用中可以扩大这些比例。
实验发现，当Mg少于0.25重量％时，如下化学反应方程式的反应不能令人满意地进行。还发现，当Mg大于18重量％时，会形成过量的Al2MgO4，从而降低接合强度。因此，Mg的范围是0.25重量％～18重量％。
对于羟基溶剂，已经发现当其少于25重量％时，上述反应不充分，同时不能形成糊状的接合剂，从而不能进行满意的涂布。还发现，当羟基溶剂大于50重量％时，因所得产物的流动性太强而不能进行成功的涂布。因此，羟基溶剂的范围是25重量％～50重量％。
参见图1，该图显示了由本发明的接合方法制造的大电流动力装置的截面图。
大电流动力装置10包括半导体元件11、支持该半导体元件11的绝缘基材12、接合到该绝缘基材12上的散热件13以及通过本发明的接合剂14接合到该散热件13上的吸热件15。
半导体元件11产生的热量传递给散热件13，再传递到吸热件15，然后散失到外部，从而可以防止半导体元件11温度上升。
下面对各组成部分的材料进行说明。
绝缘基材12由氮化铝制成。
散热件13由高导热率的铝、铜或碳化硅(SiC)制成。
吸热件15也由高导热率的铝、铜或碳化硅制成。
下面参照图2A～图2C说明具有上述结构的大电流动力装置的接合方法。
如图2A所示，准备配有半导体元件11和绝缘基材12的散热件13、吸热件15和接合剂14。
散热件13和吸热件15是不同的金属，所述散热件是铝(纯度为99.99％)，而所述吸热件是铝合金A5052(JIS：含有2.5Mg和0.25Cr的铝合金)。
为了得到接合剂14，准备50重量％的AlN粉末、10重量％的Mg粉和40重量％的水。此外，准备7倍于所述AlN粉末的量的Al粉作为添加剂，因为散热件13或吸热件15是铝或铝合金。首先，用研钵充分捏和A1N粉末(50重量％)、Mg粉(10重量％)和Al粉(7倍于所述AlN粉末)。将水(40重量％)加入捏和后的粉末中，形成含有添加剂的接合剂14。
然后如图2B所示，用接合剂14涂布散热件13。将吸热件15置于接合剂14之上。或者可将接合剂14涂布在吸热件15上。
然后如图2C所示，将其全部装入真空加热炉18，使散热件13置于两个支架16上。这样，吸热件15的重量施加给接合剂14。该负荷应产生约2MPa的压力。如果达不到2MPa的压力，则可在吸热件15上负载一重物17(如虚线所示)来补偿该压力的不足。将真空炉排空，然后在其中吹入氮气，以便制造氧浓度为3～20ppm的氮气氛。
以10℃/分钟的升温速度开始加热，升温至目标温度150℃，达到150℃后放置2小时。在此期间发生了如以下化学反应方程式所表示的反应，最终生成1120kJ的反应热。当母材或与之接合的部件是铝合金时，该反应热是使母材表面的或与之接合的部件的表面的任何致密的氧化膜发生热破坏所需热量的一部分。
8AlN+3Mg+12H2O→3Al2MgO4+2Al+8NH3-1120kJ(反应热)
从真空加热炉18取出的产品是如图1所示的动力装置10。检测动力装置10的机械性能。结果如下表所示。
 
母材 与母材接合的部件 加热温度 载荷强度 接合部厚度 拉伸强度 破坏部位
散热件(A5052) 吸热件(纯Al) 150℃ 2MPa 约100μm 约20MPa 在与母材接合的部件内
接合部的厚度也即接合剂14的厚度约为100μm，采用拉伸试验机进行拉伸破坏试验及其拉伸强度的测定。结果显示拉伸强度约为20MPa，并且在与母材接合的部件即散热件13内发生了破坏。由此证实，通过本发明的方法采用本发明的接合剂形成的接合部具有与现有产品相当的接合强度。
以下是将加热温度设定为150℃的原因。
参见图2A，采用焊料将半导体元件11固定在绝缘基材12上。由于在180℃时焊料将软化或熔化，所以如图2所示的加热必须在低于180℃的温度下进行。
由于本发明的接合剂14自身可生热，因此可以确定，通过在125℃下进行外部加热，能够得到相当于现有技术所能达到的强度。
因此，上述实施例中的温度选择为125℃到180℃的中间点150℃。
然而，由于接合强度依赖于温度，所以还需要采用180℃或高于180℃的外部加热温度来得到高强度。下面参照图3A～图3D描述一个相应的实施例。
如图3A所示，首先准备散热件13、吸热件15和接合剂14。散热件13和吸热件15是不同类型的金属，所述散热件是铝(纯度为99.99％)，而所述吸热件为铝合金A5052(含有2.5Mg和0.25Cr的铝合金)。
为了得到接合剂14，准备50重量％的AlN粉末、10重量％的Mg粉和40重量％的水。此外，由于散热件13和吸热件15分别是铝和铝合金，所以准备7倍于AlN粉末的量的Al粉作为添加剂。首先，在研钵中充分捏和AlN粉末(50重量％)、Mg粉(10重量％)和Al粉(7倍于AlN粉末)。在该捏和后的粉末中混入水(40重量％)，形成含有所述添加剂的接合剂14。
然后，如图3B所示，将接合剂14涂布到散热件13上。将吸热件15置于接合剂14之上。选择性地，也可将接合剂14涂布到吸热件15上。
然后，如图3C所示，将其全部装入真空加热炉18，使散热件13置于两个支架16上。结果，吸热件15的重量作为压力加载到了接合剂14上。此负荷应当产生约2MPa的压力。如果该负荷达不到2MPa，则在吸热件15上放置一个重物作为补偿。将真空加热炉18排空，然后向其中吹入氮气，以便制造氧浓度为3～20ppm的氮气氛。
以10℃/分钟的升温速度开始加热，升温至目标温度600℃，达到600℃后放置2小时。
最后，将散热件13从真空加热炉18中取出并反转后，用焊料等将半导体元件11和绝缘基材12接合到散热件13上。结果得到了如图3D所示的大电流动力装置。
下面参照图4A～图4C，描述将本发明的接合方法用于接合发动机部件的实施例。
参见图4A，首先准备发动机气缸21和具有翅片22的盖23。气缸21上事先附有螺栓24。气缸21由铝模铸件(JIS-ADC-12)制成，盖23也由铝模铸件(JIS-ADC-12)制成。
气缸21的上表面涂布有接合剂14。该接合剂14的组成与前述组成相同。
然后，如图4B所示，将盖23安装到气缸21上，给螺栓24装上螺母25，旋转螺母25使其将盖23紧压到气缸21上。将其压力调节为2MPa。于是，螺栓24和螺母25起到机械式千斤顶的作用。然后，将气缸21和盖23置于真空加热炉18中。将真空炉18排空，然后向其中吹入氮气，以便制造氧浓度为3～20ppm的氮气氛。
以10℃/分钟的升温速度开始加热，升温至目标温度400℃，达到400℃后放置2小时。在此期间发生了如以下化学反应方程式所表示的反应，最终生成1120kJ的反应热。当母材或与之接合的部件是铝合金时，该反应热是使母材表面的或与之接合的部件表面的任何致密的氧化膜发生热破坏所需热量的一部分。
8AlN+3Mg+12H2O→3Al2MgO4+2Al+8NH3-1120kJ(反应热)
最后，将其从真空加热炉中取出，卸掉其上的螺栓和螺母，从而得到如图4C所示的完成的气缸-盖组件20。目前通常采用螺栓来连接盖和气缸，但本发明采用了接合剂14来将两者连接在一起。
检测气缸-盖组件20的机械性能。结果如下表所示。
 
母材 与母材接合的部件 加热温度 载荷强度 接合部厚度 拉伸强度 破坏部位
气缸(ADC12) 盖(ADC12) 400℃ 2MPa 约85μm 约75MPa 在母材内
接合部的厚度也即接合剂14的厚度约为85μm，采用拉伸试验机进行拉伸破坏试验及拉伸强度的测定。结果显示拉伸强度约为75MPa，并且在母材或气缸21发生了破坏。由此证实，采用本发明的接合剂通过本发明的方法所形成的接合部具有充分的强度。
用来促进接合剂接合的外部加热温度必须为125℃或高于125℃，以便得到相当于现有技术所达到的强度。然而，鉴于必须采用比焊接温度(约640℃)低的温度以防止热变形，所以希望外部加热温度不超过600℃。因此，选择外部加热温度的范围为125℃至600℃。
此外，为了保证至少达到预定的强度，外部加热温度必须至少为150℃，而且为了充分抑制热变形，该温度必须不超过500℃。因此，外部加热温度的范围优选是150～500℃。
可以改变加入到本发明的接合剂中的所述添加剂，以便适应母材或与之接合的部件的种类。例如，如果接合面是镀Ni的，则所述添加剂为Ni粉。
下面参照图5～图9，描述采用本发明的接合方法制造气缸体的实施例。
如图5所示，首先准备由铝铸件制成的气缸体30、铝合金片34和接合剂14。下面按顺序进行详细说明。
气缸体30是具有两个邻接气缸31的铝铸件，所述的两个邻接气缸31彼此紧靠并具有狭小的气缸间隙，环绕在两个气缸31周围的两个水冷套32在与气缸盖相匹配的表面33上形成了环状开口。类似于本实施例中所述的具有彼此紧靠的邻接气缸31的结构叫做Siamese型气缸体。所述铝铸件优选具有JIS-ADC-12所规定组成的铝模铸件。
铝合金片34的厚度与限定水冷套32的空隙一致，该铝合金片可以是铸造件或压延件。
参见图6，给左侧的铝合金片34的两侧涂布接合剂14后插入到箭头所指的水冷套32中。对于右侧的铝合金片34也是如此。
参见图7，为了易于脱模，水冷套32优选是向着其开口35的方向变宽的锥形。由此，浇铸之后气缸体将易于从模具中取出。倾斜角θ1相应于铸模所形成的脱模倾斜角。
优选铝合金片34相应地具有楔形截面，该楔形截面的顶端厚度t2大于其底端厚度t1。该铝合金片的锥角记为θ2。
尽管原则上通常设定θ1＝θ2，但也有可能设定θ1<θ2。
原因如下。当θ1<θ2时，必须以强力将铝合金片34压入水冷套32。压入的结果是对接合剂14施加了作用力(压缩力)。
然后，如图8所示，将气缸体30置于真空加热炉40内。此时，通过上述楔形嵌入作用、任何其他机械夹紧力或任何其他替代方法，其对接合剂14所施加的压缩力优选约为2MPa。
开动真空泵41，对该炉进行抽真空。压力控制装置42通过压力传感器43来检测炉内压力，并使真空泵41工作，从而可以使炉压达到预定的真空度。
然后，由氮气容器44或充有氩气的惰性气体容器45等向炉内吹入气体，从而在炉内形成氧浓度为3～20ppm的氮气氛或惰性气体气氛。
然后，以10℃/分钟的升温速度开始加热，升温至目标温度400℃，达到400℃后放置2小时。温度控制装置46通过温度传感器47测定炉温并调节加热器48的给热，从而以上述加热速度使炉温升高到目标温度。
在此期间发生了如以下化学反应方程式所表示的反应，最终生成1120kJ的反应热。当母材或与之接合的部件是铝合金时，该反应热是所述母材表面的或与之接合的部件表面的致密氧化膜发生热破坏所需热量的一部分。
8AlN+3Mg+12H2O→3Al2MgO4+2Al+8NH3-1120kJ(反应热)
最后，将其从加热炉40中取出，从而得到如图9所示的完成的气缸体30。气缸体30具有多个铝合金片34，该多个铝合金片安装并由所述接合剂固定在围绕两个气缸31的水冷套32内，该水冷套32在与气缸盖相匹配的表面33上形成环状的开口。
检测铝合金片34与气缸体30之间的接合强度。结果如下表所示。
 
母材 与母材接合的部件 加热温度 载荷压力 接合部厚度 拉伸强度 破坏部位
气缸体(ADC12) 铝合金片 400℃ 2MPa 约85μm 约75MPa 在与母材接合的部件内
接合部的厚度也即接合剂14的厚度约为85μm，采用拉伸试验机进行拉伸破坏试验及其拉伸强度的测定。结果显示拉伸强度约为75MPa，并且是与母材接合的部件即铝合金片34内受到了破坏。由此证实，采用本发明的接合剂通过本发明的方法所形成的接合部具有充分的强度。
用来促进接合剂接合的外部加热温度必须为125℃或高于125℃，以便获得相当于现有技术所达到的强度。然而，鉴于必须采用比焊接温度(约640℃)低的温度以防止热变形，所以希望外部加热温度不超过600℃。因此，选择外部加热温度的范围为125℃～600℃。
此外，为了保证至少达到预定的强度，外部加热温度必须至少为150℃，而且为了充分抑制热变形，该温度必须不超过500℃。因此，优选外部加热温度的范围是150℃～500℃。
可以改变加入到本发明的接合剂中的所述添加剂，以便适应母材或与之接合的部件的种类。例如，如果接合面是镀Ni的，则所述添加剂为Ni粉。
可以将铝合金片换为装配在水冷套开口中的铝合金环。如果用接合剂涂布所述环，并将其置于水冷套的开口中加热固定，则有可能得到封闭的盖板型气缸体。开口的盖板型气缸体的铸造成本较低，但封闭的盖板型气缸体的铸造成本较高。因此，如果铸造开口的盖板型气缸体，然后采用本发明的方法将其变为封闭的盖板型气缸体，则可以降低铸造成本。
此外，尽管本发明的实施方式针对双缸式气缸体进行了描述，但该气缸体也可只具有一个气缸或具有三个甚至三个以上的气缸。本发明不仅可用于Siamese型气缸体，而且可用于非Siamese型气缸体。
工业实用性
由于本发明的接合剂及其接合方法可以满意地实现金属或陶瓷部件如发动机或大电流动力装置的接合，因此，本发明的接合剂及接合方法可用于制造发动机和电气设备。

Claims (2)

1.用于金属或陶瓷的接合剂，所述接合剂含有0.25重量％～18.0重量％的镁粉和25重量％～50重量％的水，该接合剂组成的其余部分为AlN粉末。
2.金属或陶瓷的接合方法，所述方法包括：
捏和步骤，其中，为了得到一种接合剂而对镁粉和AlN粉末进行捏和，所述接合剂含有0.25重量％～18.0重量％的镁粉和25重量％～50重量％的水，该接合剂组成的其余部分为AlN粉末；
混合步骤，其中，在即将涂布前，向上述捏和后的粉末中混入25重量％～50重量％的水；
涂布步骤，其中，用所得到的接合剂涂布金属或陶瓷母材和与之接合的部件这两方中的至少一方；
紧贴步骤，其中，采用所述接合剂使所述部件和所述母材紧贴；以及
加热步骤，其中，将保持彼此紧贴状态的所述母材和所述部件加热到150～500℃，以便促进其接合。
CNB028188888A 2001-09-27 2002-09-24 用于金属或陶瓷的接合剂以及由其接合金属或陶瓷的方法 Expired - Fee Related CN100509707C (zh)

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