CN103804009B - 陶瓷部件与金属部件之间的接合体以及其制造方法 - Google Patents
陶瓷部件与金属部件之间的接合体以及其制造方法 Download PDFInfo
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Abstract
本发明提供一种接合体及其制造方法,充分提高了将陶瓷部件和金属部件接合而得到的接合体的强度。接合体(10)在设置于板状的氧化铝或氮化铝的陶瓷部件(12)的凹部(12a)上,通过接合层(16)接合具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制的端子(14)。接合层(16)含有Au、Ge、Ag、Cu以及Ti,且与凹部(12a)的侧面的至少一部分(在这里是全部)以及底面接合。在该接合层(16)的与陶瓷部件(12)的接合界面上,Ti富集存在。另外,在将接合体(10)沿接合体(10)的厚度方向剖切时,气孔剖面面积的总和占接合层(16)剖面面积的比例(气孔率)为0.1~15%。
Description
技术领域
本发明涉及陶瓷部件与金属部件之间的接合体以及其制造方法。
背景技术
以往,作为陶瓷部件与金属部件之间的接合体,已知有金属部件的端部和陶瓷部件通过接合部来接合(专利文献1)的接合体。在该接合体中,接合部具备形成于陶瓷部件上的金属包镀层以及介于金属包镀层和金属部件的端部之间的焊料接合层。这样的接合体如下制造。即,首先,在由AlN烧结体制的圆盘状陶瓷部件的接合面上设置包含Cu-Al-Si-Ti的圆环状第1焊料。接下来,将该第1焊料在1050℃下进行5分钟的真空环境加热,形成金属包镀层。接下来,在金属包镀层上设置包含Ag-Cu的圆环状第2焊料,在其上设置筒状的金属部件的端面,在金属部件上设置配重。将其在800℃下进行5分钟的真空环境加热,形成焊料接合层。由此得到的接合体几乎没有氦漏量,即使在热循环后,没有裂纹,也几乎没有氦漏量。
现有技术文献
专利文献
专利文献1:日本特开2000-219578号公报
发明内容
但是,在这样的接合体中,得不到足够的强度。
本发明为解决上述问题而完成的,以充分提高陶瓷部件和金属部件的接合而得到的接合体的强度为主要目的。
本发明的接合体,其是通过接合层在设于氧化铝或氮化铝的陶瓷部件的凹部上,接合具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制的金属部件而得到的接合体,上述接合层含有Au、Ge、Ag、Cu以及Ti,且与上述凹部的侧面的至少一部分以及底面接合,上述接合层的与上述陶瓷部件接合的接合界面上,Ti富集存在,在将上述接合体沿上述接合体的厚度方向剖切时,气孔的剖面面积总和占上述接合层剖面面积的比例即气孔率为0.1~15%。
根据该接合体,接合陶瓷部件和金属部件而得到的接合体的强度变得足够高。对其原因进行如下推测。首先,考虑含有Au、Ge、Ag、Cu以及Ti的接合层适合于氧化铝或氮化铝的陶瓷部件与具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制金属部件之间的接合。另外,考虑是因为接合层的与陶瓷部件的接合界面上Ti富集存在,在该接合界面中Ti和陶瓷反应而接合层起到接合的作用。再有,由于气孔率为0.1~15%,因此在初期也好热循环后也好,强度均较高,而且能够防止裂纹的产生。此外,由于若气孔率未达到0.1%则产生裂纹或热循环后的强度相比于初期大幅下降,因此不优选。另外,若气孔率超过15%则强度变得极低,因此不优选。
本发明的接合体优选Ti聚集在存在于上述接合层的内部的气孔的周围。这样的Ti聚集能够从沿接合体的厚度方向剖切时的剖切面的Ti分布图像确认。
本发明的接合体的制造方法包含:
(a)准备设有凹部的氧化铝或氮化铝的陶瓷部件的工序;
(b)在上述凹部的侧面的至少一部分以及底面上涂敷Ag-Cu-Ti膏体,并在真空环境下加热至800℃~900℃,从而在上述凹部的侧面的至少一部分以及底面上形成金属包镀层的工序;以及
(c)在形成了上述金属包镀层的上述凹部的底面上设置Au-Ge薄板,在其上设置具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制的金属部件,并在真空环境下加热至360~450℃,从而在上述金属部件与上述陶瓷部件之间形成上述金属包镀层和上述Au-Ge薄板变得浑然一体的接合层的工序。
根据该接合体的制造方法,得到的接合体的强度变得足够大。另外,该制造方法适和于制造上述的接合体。
在本发明的接合体的制造方法中,在上述工序(b)中,优选将上述金属包镀层的厚度设为5~75μm。这样做的话,能够使接合体的强度变得更大。另外,能够防止在陶瓷部件产生裂纹。
在本发明的接合体的制造方法中,在上述工序(b)中,优选上述Ag-Cu-Ti膏体含有1.50~2.10wt%的Ti。若Ti的含量低于下限值,则得到的接合体的强度与初期相比在热循环后大幅下降,且热循环后会产生裂纹。另外,若Ti含量超过上限值,则得到的接合体的强度不管初期还是热循环后都变小(不产生裂纹)。
附图说明
图1是接合体10的制造工序图。
图2是将代表例的接合体沿接合体的厚度方向剖切时的剖面照片。
图中:10—接合体,12—陶瓷部件,12a—凹部,14—端子,16—接合层,20—Ag-Cu-Ti膏体,22—金属包镀层,24—Au-Ge薄板。
具体实施方式
以下,参照附图对本发明的一个优选实施方式进行说明。图1是本实施方式的接合体10的制造工序图。
如图1(d)所示,本实施方式的接合体10是如下接合体,通过接合层在设置于板状的氧化铝或氮化铝的陶瓷部件12的凹部12a上接合具有Ni覆膜、Au覆膜或Ni-Au覆膜(基底为Ni)的Mo或Ti制的端子14。接合层16含有Au、Ge、Ag、Cu以及Ti,并与凹部12a的侧面的至少一部分(在这里为全部)以及底面接合。在该接合层16的与陶瓷部件12的接合界面上,Ti富集存在。另外,在将接合体10沿接合体10的厚度方向剖切时,气孔的剖面面积的总和占接合层16的剖面面积的比例(气孔率)为0.1~15%。
此外,气孔能够作为将接合层16的剖面进行2值化处理时的暗部而求得。2值化处理,例如,能够通过对接合层16的剖面整体的像素生成亮度的直方图,直方图中出现的2个峰之间(谷)的部分的亮度值设定为阈值,将比阈值更小的亮度的像素设为0、其以上的亮度的像素设为255来进行。在下述的实施例中,以亮度值的阈值为80进行2值化处理而算出气孔率。
这样的接合体10,例如,能够如下地制造。首先,准备具有凹部12a的陶瓷部件12(参照图1(a))。接下来,在凹部12a的侧面的至少一部分以及底面上涂敷Ag-Cu-Ti膏体20,涂敷结束后进行干燥,通过在真空环境下加热至800~900℃来进行烧镀(参照图1(b))。其结果为,在凹部12a的侧面的至少一部分以及底面上形成了金属包镀层22。由于在烧镀时若温度未满800℃则膏体材料的反应性变差而不优选,若超过900℃,则因反应生成物增加,热膨胀差的增加或杨氏模量的增加而残余应力变大,成为产生裂纹或强度变低的原因而不优选。接下来,在形成了金属包镀层22的凹部12a的底面上设置Au-Ge薄板24(参照图1(c))。然后,在Au-Ge薄板24上搭载端子14,在端子14上搭载未图示的配重,以该状态在真空环境加热至360~450℃。由此,金属包镀层22和Au-Ge薄板24变得浑然一体的接合层16形成于端子14和陶瓷部件12之间。其结果为,得到接合体10(参照图1(d))。若加热时的温度未满360℃,则由于焊料(Au-Ge薄板)的反应性变差而不优选,如超过450℃,则因反应生成物增加,热膨胀差的增加或杨氏模量的增加而残余应力变大,成为产生裂纹或强度变低的原因而不优选。
根据以上说明的接合体10,接合陶瓷部件与金属部件的接合体的强度变得足够高。对其理由进行以下的推测。首先,考虑含有Au、Ge、Ag、Cu以及Ti的接合层16适合于陶瓷部件12和端子14之间的接合。另外,考虑因为在接合层16的与陶瓷部件12的接合界面上Ti富集存在,所以在该接合界面上Ti和陶瓷反应而起到使接合层16与陶瓷部件12较强接合的作用。再有,由于气孔率为0.1~15%,因此不管在初期还是热循环后强度均较高,而且能够防止裂纹产生。
此外,本发明并不限定于上述的实施方式,当然可以在属于本发明的技术范围内通过种种形态来实施。
例如,在上述实施方式中,也可以使用在内部埋设有电极的陶瓷部件12,在凹部12a的底面上预先露出与该电极连接的导电部件,并将端子14通过接合层16接合至该导电部件。在该情况下,端子14用于给电极供电。此外,作为电极,例如可以举出加热电极(电阻发热体)或静电吸盘用电极、等离子产生用电极等。
[代表例]
准备设置有直径6mm、深度0.5mm的凹部(端子孔)的氧化铝陶瓷部件。对该氧化铝陶瓷部件的凹部的周围用掩模带进行掩模,在该凹部的侧面以及底面上由分配装置涂敷Ag-Cu-Ti膏体。涂敷结束后,自然放置10分钟,随后,用洁净烘干炉以120℃(物体温度)干燥1小时。揭下掩模带,在烧成温度850℃、烧成时间10分钟、真空度5×10-5Torr以下的条件下进行烧镀。由此,在凹部的侧面以及底面上形成Ag-Cu-Ti的金属包镀层。金属包镀层的膜厚为30μm。此外,Ag-Cu-Ti膏体的Ti含量为1.7wt%。
随后,在凹部的底面上设置直径5.5mm、厚度0.15±0.05mm的Au-Ge薄板。在其上设置具有Ni覆膜的Mo制端子(直径5.8mm、厚度6mm),搭载配重后进行水平校准以及位置对准。随后,以烧制温度400℃、烧制时间10分钟、真空度5×10-5Torr以下的条件进行处理。由此,得到金属包镀层和Au-Ge薄板变得浑然一体的接合层形成于端子和氧化铝陶瓷部件之间的接合体。接合层与凹部的侧面以及底面相接合。
接合层的构成元素用EMPA进行解析,含有Au、Ge、Ag、Cu以及Ti。另外,在接合层的与氧化铝陶瓷部件的接合界面上,Ti富集存在。具体来说,从将接合体沿接合体的厚度方向剖切的剖面的Ti分布图像观察,能够观察到在氧化铝陶瓷部件和接合层之间的界面上存在Ti层,Ti在气孔周边的凝集。之所以在氧化铝陶瓷部件和接合层之间的界面上存在Ti层,考虑是因为Ti和氧化铝反应,该Ti层起到将氧化铝陶瓷部件和接合层接合的作用。再有,在接合层上分布有较小的气孔,气孔率为5.3%。气孔率是对接合层的剖面进行2值化处理时,将暗部看作气孔的剖面,气孔的剖面面积的总和相比于接合层的剖面面积的比例。图2表示接合层的剖面照片。2值化处理使用HALCON11.0来进行(HALCON是MVTec Software GmbH的注册商标)。
[金属包镀层的膜厚]
在上述的代表例中,以在凹部形成金属包镀层时的膜厚成为表1所示的值的方式制作接合体。测定制作的接合体的断裂强度,并且检查是否在接合之后的接合体的氧化铝陶瓷部件上观察到裂纹。用表1表示其结果。此外,断裂强度与拉伸断裂负载是一个意思,以氧化铝陶瓷部件处于下方的方式将接合体可靠地固定于支撑台,使其不能在上下方向上移动,向从端子的上面垂直向下地设置的螺栓孔内拧入拉伸棒的前端,在该拉伸棒上加载垂直向上的负载,将接合层断裂时的负载记作断裂强度。
在表1中,裂纹的指标定义为,○:没观察到裂纹,△:虽然能观察到裂纹但是程度轻微,对接合特性没有影响,×:观察到裂纹,会带来致命的影响。
(表1)
从表1可以明确看出,在形成于凹部的金属包镀层的膜厚为2~80μm的情况下,断裂强度高达50kgf以上,也观察不到裂纹。特别是其膜厚为5~75μm时,断裂强度变得更高(120kgf以上)。此外,在上述的代表例中,代替涂敷Ag-Cu-Ti膏体而使用Ag-Cu-Ti薄板仅在底面形成金属包镀层时,即使金属包镀层的膜厚为25μm也观察到裂纹。从以上可以看出,金属包镀层有必要不仅形成于凹部的底面还有必要形成于侧面的至少一部分。另外,可以看出金属包镀层的膜厚为2~80μm、优选为5~75μm时,断裂强度较高也观察不到裂纹。若金属包镀膜厚低于到2μm,则形成于氧化铝陶瓷部件的金属包镀层不充分而强度下降,相反地若金属包镀膜厚超过80μm则发生裂纹强度下降。此外,在金属包镀层的膜厚为2~80μm的情况下,接合层和氧化铝陶瓷部件之间的接合层上Ti富集存在。
[气孔率]
在上述的代表例中,以调整Ag-Cu-Ti膏体中的Ti含量而制作接合体,使气孔率为表1所示的0~35%。测定刚制作完成的接合体的断裂强度和有无裂纹。另外,测定热循环试验后的接合体的断裂强度和有无裂纹。热循环试验为,将从室温加热至200℃后再冷却至室温的操作作为1次循环,反复进行1000次循环。其结果表示在图2中。
此外,对使用Ti含量为0%的膏体的例子进行一次测定,对使用Ti含量0.5%、1.5%的膏体的例子各进行2次的测定,对使用其余的膏体的例子各进行3次的测定。
在表2中,裂纹的指标定义为,○:没观察到裂纹,△:虽然能观察到裂纹但是程度轻微,对接合特性没有影响,×:观察到裂纹,会带来致命的影响。
(表2)
从表2可以明确看出,具有气孔率为0.1~15%的接合层的接合体(主要使用Ti含量为1.50~2.10wt%的Ag-Cu-Ti膏体而制造的接合体)在初期以及热循环后断裂强度都高达120kgf以上,在初期以及热循环后都观察不到裂纹。另外,在具有气孔率为0.1~15%的接合层接合体中,与代表例一样,接合层和氧化铝陶瓷部件之间的接合界面上Ti富集存在。再有,在气孔率为0.1~15%的接合层中,已确认与代表例一样含有Au、Ge、Ag、Cu以及Ti。
另外,在上述的代表例中,使用氮化铝陶瓷部件代替氧化铝陶瓷部件、使用具有Au覆膜的Mo端子代替具有Ni覆膜的Mo端子、且除Ag-Cu-Ti膏体的Ti含量为1.8wt%以外,与上述的代表例一样地的制作接合体。此外,金属包镀层的厚度为30μm。该接合体也是在端子和陶瓷部件之间形成有金属包镀层和Au-Ge薄板变得浑然一体的接合层。另外,在该接合层的与陶瓷部件的接合界面上Ti富集存在。气孔率为4.1%。对该接合体,刚制作完成时的断裂强度和热循环试验后的断裂强度分别为147kgf、144kgf,具有足够的强度。另外,在刚制作完成时和热循环试验后都观察不到裂纹。能得到这样的结果的原因能列举出,氮化铝陶瓷也和氧化铝陶瓷一样,在接合层和陶瓷部件的接合界面上Ti富集存在,另外对于Au覆膜,其与接合层的润湿性和Ni覆膜一样好。
另外,在上述的代表例中,使用具有Ni覆膜的Ti端子代替具有Ni覆膜的Mo端子、且除Ag-Cu-Ti膏体的Ti含量为1.8wt%以外,与上述的代表例一样地的制作接合体。此外,金属包镀层的厚度为30μm。该接合体也在端子和陶瓷部件之间形成由金属包镀层和Au-Ge薄板变得浑然一体的接合层。另外,在该接合层的与陶瓷部件的接合界面上Ti富集存在。气孔率为3.8%。对该接合体,刚制作完成时的断裂强度和热循环试验后的断裂强度分别为148kgf、146kgf,具有足够的强度。另外,在刚制作完成时和热循环试验后都观察不到裂纹。
Claims (5)
1.一种接合体,其是通过接合层在设于氧化铝或氮化铝的陶瓷部件的凹部上,接合具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制的金属部件而得到的接合体,上述接合体的特征在于,
上述接合层含有Au、Ge、Ag、Cu以及Ti,且与上述凹部的侧面的至少一部分以及底面接合,
上述接合层的与上述陶瓷部件接合的接合界面上,Ti富集存在,
在将上述接合体沿上述接合体的厚度方向剖切时,气孔的剖面面积总和占上述接合层剖面面积的比例,即气孔率为0.1~15%。
2.根据权利要求1所述的接合体,其特征在于,
Ti聚集在存在于上述接合层的内部的上述气孔的周围。
3.一种接合体的制造方法,上述接合体为权利要求1或2所述的接合体,其特征在于,包含以下工序:
(a)准备设有凹部的氧化铝或氮化铝的陶瓷部件的工序;
(b)在上述凹部的侧面的至少一部分以及底面上涂敷Ag-Cu-Ti膏体,并在真空环境下加热至800℃~900℃,从而在上述凹部的侧面的至少一部分以及底面上形成金属包镀层的工序;以及
(c)在形成了上述金属包镀层的上述凹部的底面上设置Au-Ge薄板,在其上设置具有Ni覆膜、Au覆膜或基底为Ni的Ni-Au覆膜的Mo或Ti制的金属部件,并在真空环境下加热至360~450℃,从而在上述金属部件与上述陶瓷部件之间形成上述金属包镀层和上述Au-Ge薄板变得浑然一体的接合层的工序。
4.根据权利要求3所述的接合体的制造方法,其特征在于,
在上述工序(b)中,上述金属包镀层的厚度设为5~75μm。
5.根据权利要求3或4所述的接合体的制造方法,其特征在于,
在上述工序(b)中,上述Ag-Cu-Ti膏体含有1.50~2.10wt%的Ti。
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