CN103502787A - 陶瓷压力测量单元及其制造方法 - Google Patents

陶瓷压力测量单元及其制造方法 Download PDF

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CN103502787A
CN103502787A CN201280013585.XA CN201280013585A CN103502787A CN 103502787 A CN103502787 A CN 103502787A CN 201280013585 A CN201280013585 A CN 201280013585A CN 103502787 A CN103502787 A CN 103502787A
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brazing
hard solder
active hard
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film
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CN103502787B (zh
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武尔费特·德鲁斯
安德烈亚斯·罗斯贝格
埃尔克·施密特
安德烈·贝林格尔
拉尔夫·尤林
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Endress and Hauser SE and Co KG
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Abstract

本发明涉及一种用于制造压力传感器1的方法，该压力传感器包括陶瓷主体2和陶瓷测量膜3，其中，利用活性硬焊料4使测量膜与主体压力密闭地接合，其中，该方法包括：提供主体2和测量膜3和活性硬焊料4；将活性硬焊料定位在主体与测量膜之间；利用激光器10通过辐照活性硬焊料来熔化活性硬焊料，其中，穿过测量膜辐照活性硬焊料；以及通过冷却使活性硬焊料硬化。

Description

陶瓷压力测量单元及其制造方法
技术领域
本发明涉及一种陶瓷压力测量单元及其制造方法。
背景技术
本发明领域的陶瓷压力测量单元包括：陶瓷平台和陶瓷测量膜，其中平台和测量膜沿着周围接缝彼此接合使得在平台与测量膜之间形成测量腔室，其中接头包括活性硬焊料或铜焊。用于测量膜和平台的建立的陶瓷材料为刚玉，其中作为活性硬焊料或铜焊，特别地使用Zr63Ni22Ti15活性硬焊料或铜焊。
为了接合部件，它们被布置在高真空烤箱中相对于彼此所希望的位置并且被加热直到活性硬焊料或铜焊在900℃熔化并且主动地形成与陶瓷的结合。在熔化之后，允许压力测量单元在炉中在真空下冷却并且在给定情况下，有时添加保护气体。
根据对焊料执行的量热测量，已知液相线温度处在约860℃并且固相线温度在约800℃。来自熔体的相的结晶出现在这个温度范围。低于固相线温度可能形成其它相。已知总是相同的热力学相形成。
对于穿过接头的截面利用反射式电子显微术（REM）进行的研究已经确定不同偏析相占据接头内较大区域。由于这涉及到具有不同组成的相，假定它们性质不同，例如热膨胀系数、压缩或拉伸强度。因此，接头的品质在强度、密封和/或成品率方面降级。
发明内容
因此，本发明的目的在于提供一种具有改进的接头的压力测量单元及其制造方法。
根据本发明，通过独立专利权利要求1中限定的方法和根据独立专利权利要求14中限定的压力测量单元来实现这个目的。
用于制造压力测量单元的本发明的方法，该压力测量单元具有陶瓷平台和陶瓷测量膜，其中利用活性硬焊料或铜焊使测量膜与平台压力密闭地接合，该方法包括：提供平台、测量膜和活性硬焊料或铜焊；将活性硬焊料或铜焊放置于平台与测量膜之间；利用激光器辐照活性硬焊料或铜焊来熔化活性硬焊料或铜焊，其中穿过测量膜辐照活性硬焊料或铜焊；以及通过冷却使活性硬焊料或铜焊凝固。
在本发明的进一步发展中，熔化的活性硬焊料或铜焊被保持在液相线温度或高于液相线温度不超过1分钟，特别地不超过30秒，优选地不超过15秒。
液相线温度为高于该温度活性硬焊料或铜焊完全为液体因此不再包含固相的温度。
在本发明的进一步发展中，以不小于20K/min，特别地不小于40K/min，优选地不小于1K/s，并且特别优选地不小于2K/s的平均冷却速率通过冷却使活性硬焊料或铜焊凝固直到固相线温度。
固相线温度为低于该温度活性硬焊料或铜焊不再包含液相的温度。
在本发明的进一步发展中，以不小于20K/min，特别地不小于40K/min，优选地不小于1K/s，并且特别优选地不小于2K/s的平均速率冷却直到低于固相线温度100k，优选地低于固相线温度200K。
在本发明的进一步发展中，通过向压力测量单元提供稀有气体，特别是氩气来支持冷却。
本发明是从以下构思发展而来：通过利用激光器辐照来对活性硬焊料或铜焊进行局部加热，热输入如此小使得熔体能够快速冷却。那么存在更少的时间可用于接头中成核和偏析相生长，使得偏析相（就它们存在的程度而言）更小并且因此对于接头的行为起到更少的决定性作用。
在本发明的进一步发展中，以一定波长利用激光器辐照活性焊料，在这个波长，测量膜的陶瓷材料并不吸收或至多可忽略地吸收，其中该波长特别地处在可见区域中。当在测量膜的上表面进入测量膜内的光强度的至少90%，特别地至少95%到达平行于上表面的测量膜的下表面时，特别地存在在本发明的意义上的可忽略的吸收，其中下表面特别地为接触活性硬焊料或铜焊的表面。
在本发明的进一步发展中，平台和测量膜被完全加热，但至少在接头区域中被局部地加热到一定温度，该温度低于活性硬焊料或铜焊的固相线温度不超过200K，特别地低于活性硬焊料或铜焊的固相线温度不超过100K并且优选地低于活性硬焊料或铜焊的固相线温度不超过50K。
但是平台和测量膜应在任何情况下都不预热到活性硬焊料或铜焊的液相线温度并且根据本发明的进一步发展，并不超过活性硬焊料或铜焊的固相线温度。
在本发明的进一步发展中，利用在一定波长范围的激光器特别地利用Nd-YAG激光器或CO2激光器来进行预热，在该波长范围，平台或者测量膜的陶瓷材料吸收。
在本发明的进一步发展中，利用烤箱进行预热，部件布置于烤箱中。
在本发明的进一步发展中，活性硬焊料或铜焊的熔化或者使活性硬焊料或铜焊凝固，至少有时在真空和/或保护气体特别是氩气下进行。
在本发明的进一步发展中，平台和测量膜的陶瓷材料包括刚玉。
在此情况下，测量膜可特别地包括可用于该平台的更高纯度和更高极限拉伸强度的刚玉。在本发明的进一步发展中，测量膜包括高纯度Al2O3陶瓷，其特别地特征在于在可见波长范围中很低密度的散射中心，使得测量膜的陶瓷材料在此波长范围是基本上透明的。因此，能特别容易地穿过测量膜受控制地辐照活性硬焊料或铜焊。
例如在专利文献DE102008036381B3中公开了适合于用作膜材料的相对应的陶瓷材料。
在本发明的进一步发展中，测量膜的材料可具有横向断裂应力σc，其分布F(σc)由威布尔参数σ0≥500MPa，特别地σ0≥650MPa，优选地σ0≥800MPa和m≥24给出，并且烧结材料的平均粒度不超过2μm，优选地不超过1.75μm和特别优选地不超过1.5μm。
正是对于这些高强度测量膜，用于接合测量膜的本发明的方法是至关重要的。因此，本发明改进了接头的强度，并且因此，在测量膜与接头之间存在相对应性。
特别地根据本发明的方法可得到的本发明的压力测量单元，包括：陶瓷平台和陶瓷测量膜，其中利用周围接头来连接测量膜与平台的表面以在平台的表面与测量膜之间形成测量腔室，其中接头包括活性硬焊料或铜焊，其中，就接头包含活性硬焊料或铜焊的任何偏析、特别地颗粒偏析相的程度而言，这些相，特别地颗粒偏析相在垂直于平台表面的方向上具有不超过4μm，特别地不超过2μm和优选地不超过1μm的最大范围。
根据本发明，压力测量单元的陶瓷测量膜和陶瓷平台包括刚玉，其中活性硬焊料或铜焊包括Zr-Ni-Ti活性硬焊料或铜焊，或者Cu-Ti-Zr-Ni活性硬焊料或铜焊。
在Zr-Ni-Ti活性硬焊料或铜焊的目前优选的实施例中，例如具有以下组成：Zr63%、Ni22%和Ti15%。在Cu-Ti-Zr-Ni活性硬焊料或铜焊的目前优选的实施例中，其具有以下组成：Cu47%、Ti34%、Zr11%、Ni8%。在此段落中所有%数据为原子%。
本发明的压力测量单元可为绝对、相对或压差测量单元。
本发明的压力测量单元还包括换能器，用于将测量膜的压力有关的变形换能为信号，特别是电信号或光信号。目前，电容换能器优选地为电换能器，其中，为此，测量膜和平台在其界定测量腔室的表面上具有电极，并且其中在电极之间的电容为压力相关的。
附图说明
现将基于附图来解释本发明，本发明的视图如下所示：
图1为本发明的领域的压力测量单元的纵截面图；
图2为本发明的领域的压力测量单元的接头的纵截面图；以及
图3为在根据本发明的方法在制造期间本发明的压力测量单元的图示。
具体实施方式
图1所示的陶瓷压力测量单元1包括刚玉的圆柱形平台2，其具有例如1至7cm的直径和3mm至3cm的高度。高纯度刚玉的测量膜3经由环形包围接头4被压力密闭地接合到平台，其中接头4包括活性硬焊料或铜焊，特别地是Zr-Ni-Ti活性硬焊料或铜焊。接头4的高度预先决定在测量膜与平台之间的间隔，其中该间隔可为例如10μm至80μm。环形接头4的宽度，即在内半径与外半径之间的差异，总计为数mm。在测量膜3与平台2之间形成由接头4包围的测量腔室5，其中相对于在测量腔室中的压力进行压力测量，其中待测量的压力作用于背向测量腔室5的测量膜的侧部上。测量膜的厚度取决于其直径和所期望的测量范围。该厚度可例如在50μm至3mm的范围。
图2为穿过具有例如30μm厚度的接头的纵截面的更大放大的示意图，例如在本发明领域的压力测量单元的情况下存在。附图基于REM照片。在平台2与测量膜3之间的接头4具有不同的结构，其中，某些颗粒偏析相具有大于10μm的直径。不同的影线将不解释为指示独特限定相；而是，其仅示出了多个颗粒偏析相存在于可能非晶基质中。图示的大小分布直接对应于观察。为了缩短成核和偏析相生长的时间，根据本发明的方法制造压力测量单元，例如现将基于图3进行解释。
在刚玉的平台2上布置活性硬焊料或铜焊的环4，其中该环优选地呈焊料预成型体的形式。在本发明的进一步发展中，但该环也可至少部分地由在平台2上的气相沉积提供。
然后，高纯度刚玉的测量膜3放置于焊料环4上，其中测量膜3首先在可见光谱范围几乎不吸收，并且其次几乎不具有任何散射中心。
利用CO2激光器或另外合适激光器10从压力测量单元的上侧穿过测量膜3辐照活性硬焊料或铜焊4，其中，优选地，仅辐照轮廓线7外侧测量膜面的外边缘区域6，其中由活性硬焊料或铜焊环4的内半径限定轮廓线7，并且其中撞击测量膜3的外边缘区域6的激光器10的射线穿过测量膜3并且撞击活性硬焊料或铜焊的环4，以便加热它。
激光束可特别地以光栅图案移动和/或脉动。
活性硬焊料或铜焊的温度可特别地通过高温测量来监视。
利用Nd-YAG激光器等等，独立于活性硬焊料或铜焊的辐照，可将平台和测量膜加热到接近活性硬焊料或铜焊的固相线温度的温度。能够同样通过高温测量进行平台温度和测量膜温度的监视。
将平台和测量膜加热到例如活性硬焊料或铜焊的固相线温度导致在活性硬焊料或铜焊凝固时，限制了在焊料与陶瓷部件之间的机械应力。
在活性硬焊料或铜焊已经到达液相线温度使之熔化后，可以开始冷却，由于与现有技术相比更少的引入热量，所以能够更快地进行冷却。因此，更快地经过能出现成核和偏析相生长的温度范围。因此，能显著地减小这样的偏析、特别是颗粒相的大小。
优选地在不超过5×10-6mbar的压力的真空下进行测量膜与平台的接合。为了冷却，可以将氩气引入到真空设备内以便提高冷却速率。

Claims (14)

1.一种制造压力测量单元的方法，所述压力测量单元具有陶瓷平台和陶瓷测量膜，其中，利用活性硬焊料或铜焊使所述测量膜与所述平台压力密闭地接合，其中，所述方法包括：
提供所述平台、所述测量膜和所述活性硬焊料或铜焊；
将所述活性硬焊料或铜焊定位在所述平台与所述测量膜之间；
利用激光器辐照所述活性硬焊料或铜焊来熔化所述活性硬焊料或铜焊，其中，穿过所述测量膜辐照所述活性硬焊料或铜焊；以及
通过冷却使所述活性硬焊料或铜焊凝固。
2.根据权利要求1所述的方法，其中，所述熔化的活性硬焊料或铜焊被保持在所述液相线温度或高于所述液相线温度不超过1分钟，特别地不超过30秒，优选地不超过15秒。
3.根据权利要求1或2所述的方法，其中，以不小于20K/min，特别地不小于40K/min，优选地不小于1K/s，并且特别优选地不小于2K/s的平均冷却速率通过冷却使所述活性硬焊料或铜焊凝固直到固相线温度。
4.根据权利要求3所述的方法，其中，以不小于20K/min，特别地不小于40K/min，优选地不小于1K/s，并且特别优选地不小于2K/s的平均速率进一步冷却直到低于固相线温度100K，优选地低于所述固相线温度200K的温度。
5.根据前述权利要求中任一项所述的方法，其中，通过向所述压力传感器提供稀有气体，特别是氩气来支持所述冷却。
6.根据前述权利要求中任一项所述的方法，其中，利用一定波长的激光器来辐照所述活性焊料，在所述波长所述测量膜的所述陶瓷材料并不吸收或至多可忽略地吸收，其中，所述波长特别地处在可见区域中。
7.根据前述权利要求中任一项所述的方法，其中，所述平台和所述测量膜在所述接头区域中被至少局部地加热到一定温度，所述温度低于所述活性硬焊料或铜焊的固相线温度不超过200K，特别地低于所述活性硬焊料或铜焊的固相线温度不超过100K并且优选地低于所述活性硬焊料或铜焊的固相线温度不超过50K。
8.根据权利要求7所述的方法，其中，利用一定波长范围的激光器特别地利用Nd-YAG激光器或CO2激光器来进行所述预热，在所述波长范围中所述平台或者所述测量膜的所述陶瓷材料吸收。
9.根据权利要求7或8所述的方法，利用烤箱进行所述预热，所述部件布置于所述烤箱中。
10.根据前述权利要求中任一项所述的方法，其中，所述活性硬焊料或铜焊的熔化或者使所述活性硬焊料或铜焊凝固至少有时在真空和/或保护气体，特别是氩气下进行。
12.根据前述权利要求中任一项所述的方法，其中，所述平台和所述测量膜的所述陶瓷材料包括刚玉。
13.根据前述权利要求中任一项所述的方法，其中，所述测量膜的所述陶瓷材料是基本透明的。
14.特别地根据前述权利要求中任一项所述的方法可得到的压力测量单元，所述压力测量单元包括：陶瓷平台和陶瓷测量膜，其中，利用周围接头来连接所述测量膜与所述平台的表面以在所述平台的所述表面与所述测量膜之间形成测量腔室，其中，所述接头包括活性硬焊料或铜焊，其中，就所述接头包含所述活性硬焊料或铜焊的任何偏析，特别地颗粒偏析相的程度而言，这些偏析相在垂直于所述平台的所述表面的方向上具有不超过4μm，特别地不超过2μm和优选地不超过1μm的最大范围。
15.根据权利要求14所述的压力测量单元，其中，所述陶瓷测量膜和所述陶瓷平台包括刚玉，并且其中，所述活性硬焊料或铜焊包括Zr-Ni-Ti活性硬焊料或铜焊，或者Cu-Ti-Zr-Ni活性硬焊料或铜焊。
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