CN109641800A - 多孔材料、用于生产多孔材料的粉末、生产多孔材料的方法和组件 - Google Patents
多孔材料、用于生产多孔材料的粉末、生产多孔材料的方法和组件 Download PDFInfo
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Abstract
本发明涉及一种多孔材料,特别是传感器用铸造化合物,其中,根据本发明,所述多孔材料,特别是所述铸造化合物在1000℃的温度下具有至少105Ω·cm,特别是至少106Ω·cm的比电阻。
Description
本发明涉及一种多孔材料,特别是一种传感器用铸造化合物。本发明还涉及一种用于生产多孔材料的粉末,其包括金属氧化物粒子,特别是氧化铝粒子(Al2O3本发明)和/或氧化镁粒子(MgO)和/或氧化铍粒子(BeO)。此外,本发明涉及一种生产多孔材料的方法,特别是根据本发明的多孔材料。此外,本发明涉及一种具有涂层和/或包埋于铸造化合物中的组件,其中一或多种涂层和/或铸造化合物是根据本发明的多孔材料或根据本发明生产的多孔材料。
必须保护传感器免受化学侵蚀性//腐蚀性环境的影响。例如,必须保护汽车排气管线中的传感器免受化学侵蚀性环境的影响。包埋于壳体中的传感器必须另外满足耐腐蚀性和/或耐热冲击性和/或耐振动性的要求。
基于磷酸盐水泥的铸造化合物是从最新技术中得知的。然而,此类铸造化合物在高温下的导电性增加。此外,磷酸盐水泥具有化学反应性。
另外,众所周知,传感器所在的壳体可能是粉末状的。此类传感器实施例的一个缺点是耐热冲击性和耐振动性不足。
本发明的目的是提供进一步研发的多孔材料,特别是传感器用铸造化合物。多孔材料(特别是铸造化合物)应以使多孔材料(特别是铸造化合物)在高温下具有电绝缘效果的方式进行改进。另外,多孔材料,特别是铸造化合物应对热冲击和振动具有抗性。多孔材料,特别是铸造化合物应优选适合在传感器壳体内使用,其中传感器优选为铂薄膜传感器。
另外,本发明的另一目的是提供一种用于生产多孔材料,特别是用于生产铸造化合物的粉末。本发明的另一目的是提供一种生产多孔材料,特别是传感器用铸造化合物的进一步研发的方法。此外,本发明的另一目的是提供一种具有涂层和/或包埋于铸造化合物中的进一步研发的组件,其中一或多种涂层和/或铸造化合物根据本发明进一步研发。
通过权利要求1的特征,根据本发明实现了关于多孔材料的这一目的。关于用于生产多孔材料的粉末,此目的通过权利要求7的特征来实现。关于生产多孔材料的方法,此目的通过权利要求11的特征来实现。关于具有涂层和/或包埋于铸造化合物中的组件,此目的通过权利要求18的特征来实现。
本发明基于提供多孔材料,特别是传感器用铸造化合物的构思,其中多孔材料,特别是传感器用铸造化合物在1000℃的温度下的比电阻达到至少105Ω·cm,特别是至少106Ω·cm。
多孔材料,特别是传感器用铸造化合物的比电阻(RS)优选通过使用根据ASTMD257-07标准的4点测量或2点测量来确定。为此,例如,提供尺寸为20mm×60mm的衬底,例如玻璃。将待测试的多孔材料,特别是传感器用铸造化合物施加到衬底上。各端设有扁平金属条。例如,金属条彼此平行布置,其中间距为10mm。电流源(Keithley2000)连接到两个触点并预先选择电流值。
在4点测量的情况下,使用压在金属条上的两个测试尖端和电位计(Hewlett-Packard4355A)测量金属条之间的电势降,并确定表面电阻(surface resistance,SR)。在平行生产的层上确定层厚度(d)。以下等式用于比电阻:RS=SR·d。
特别地,铸造化合物不是液体铸造化合物。铸造化合物也可以称为铸造组合物,特别为已经铸造的物质。铸造化合物优选在至少部分固化和/或干燥的状态下。在本发明的特别优选的实施例中,铸造化合物是陶瓷铸件。
铸造化合物在1000℃的温度下的高比电阻意味着,例如,即使在排气管线中普遍的高温下,传感器仍会产生精确的测量值。
多孔材料可包括金属氧化物,特别是氧化铝(Al2O3)和/或氧化镁(MgO)和/或氧化铍(BeO)。
多孔材料的特征优选在于孔相互连接并形成渗滤***。此类金属氧化物或此类金属氧化物的混合物相对于铂是化学中性的,因此本发明多孔材料可特别用作铂传感器用铸造化合物。
多孔材料可包括高纯度氧化铝,其中氧化铝(Al2O3)的纯度程度达到至少99.99%。多孔材料尤其优选仅由高纯度氧化铝(Al2O3)组成,其中氧化铝(Al2O3)的纯度程度达到至少99.99%。此类纯氧化铝确保了非常好的电绝缘。
以多孔材料的总重量计,多孔材料的碳(C)含量优选小于1000ppm,特别小于500ppm,特别小于250ppm,特别小于100ppm。
另外,以多孔材料的总重量计,选自由以下组成的群组的一种元素:
锂(Li)、钠(Na)、钾(K)、硼(B)、硅(Si)、锗(Ge)、锡(Sn)、铅(Pb)、铟(In)、铊(Tl)、磷(P)、砷(As)、锑(Sb)、铋(Bi)、硫(S)、硒(Se)、碲(Te)、锌(Zn)、镉(Cd)、银(Ag)和汞(Hg)
的量占小于100ppm。以多孔材料的总重量计,前述群组中的几种元素优选构成小于1000ppm的总量。换句话说,选自上述群组的个别元素的量小于100ppm。如果存在几种选自上述群组的元素,则以多孔材料的总重量计,所有元素的总和的量小于1000ppm。
材料的孔隙率D优选为25%至50%。多孔材料的孔体积优选为0.05cm3/g至0.5cm3/g。在尤其优选的实施例中,孔隙率尤其优选为35%,孔体积为0.14cm3/g。
孔隙度和/或孔体积优选通过汞孔隙率测定法来确定。优选使用来自Porotec公司的设备进行汞孔隙率测定(低压范围中的140帕斯卡,高压范围中的440帕斯卡)。根据DIN66133标准,通过压汞确定固体的孔体积分布和比表面积。在测量之前,多孔材料的各层优选在200℃下加热约1小时。
多孔材料可另外具有50至150nm的孔径d50。换句话说,孔径的d50值(中值)可为50至150nm。在特别优选的具体实施例中,孔径的d50值为88nm。
孔径,特别是d50值(中值)的确定优选通过如已描述的汞孔隙率测定法来执行。另外,能够通过显微法确定这一值。
多孔材料的热膨胀系数可以在6·106/K至15·106/K的范围内。换句话说,多孔材料的热膨胀系数优选为6.5·106/K至15·106/K。在本发明的另一具体实施例中,热膨胀可以达到6.5·106/K至8.5·106/K。例如,通过膨胀测定法来确定热膨胀。
另外,多孔材料的3点弯曲强度优选为20N/mm2。在本发明的特别优选的具体实施例中,3点弯曲强度为46N/mm2。
特别体现为传感器用铸造化合物的多孔材料结合了几个优点。因此,多孔材料提供了非常好的电气安装。此外,多孔材料具有高强度。多孔材料的多孔微结构另外允许向传感器供氧。此外,多孔材料相对于铂是化学中性的,并且吸收例如可以从保护套管中发出的金属和金属氧化物蒸汽。
由于所用材料的纯度,特别是所用铝的纯度,实现了传感器,特别是铂传感器的较低中毒。由于材料的多孔性,可以实现过滤功能。
多孔材料,特别是传感器用铸造化合物,特别是烧制或烧结材料。
本发明的另一方面涉及用于生产多孔材料的粉末。特别地,本发明的这一方面涉及用于生产根据本发明的多孔材料的粉末。所述粉末包括金属氧化物粒子,特别是氧化铝粒子(Al2O3)和/或氧化镁粒子(MgO)和/或氧化铍粒子(BeO)。
根据本发明,粉末包括至少两个粒子级分(particle fraction),特别是至少三个粒子级分,其中各粒子级分的粒度d50具有不同值。
粒度d50为中值。
在特别优选的具体实施例中,粉末具有高纯度氧化铝(Al2O3),其中氧化铝(Al2O3)的纯度程度为至少99.99%。在本发明的具体实施例中,仅由高纯度氧化铝(Al2O3)组成的粉末同样是极其优选的,其中氧化铝(Al2O3)的纯度程度为至少99.99%。
以粉末的总重量计,粉末的碳含量优选小于1000ppm,特别小于500ppm,特别小于250ppm,特别小于100ppm。
粉末可含有额外的元素,其中以多孔材料的总重量计,元素的量选自由以下组成的群组:
锂(Li)、钠(Na)、钾(K)、硼(B)、硅(Si)、锗(Ge)、锡(Sn)、铅(Pb)、铟(In)、铊(Tl)、磷(P)、砷(As)、锑(Sb)、铋(Bi)、硫(S)、硒(Se)、碲(Te)、锌(Zn)、镉(Cd)、银(Ag)和汞(Hg)
达到小于100ppm。以多孔材料的总重量计,前述群组中的几种元素优选构成小于1000ppm的总量。换句话说,选自上述群组的每个单独元素的量小于100ppm。如果存在几种选自上述群组的元素,则以多孔材料的总重量计,所有元素的总量将合计小于1000ppm。
通过发射光谱测定法确定粉末,特别是(Al2O3)粉末的纯度。将来自赛默飞世尔科技(ThermoFisher Scientific)的iCAP 6500duo模型或iCAP 7400duo模型的ICP分光仪用于测量。
根据DIN EN ISO 11885标准进行测量。在氧化铝(Al2O3)粉末的情况下,将100mg样品与8mL盐酸(HCl)、2mL硝酸(HNO3)和1.5mL氟化氢(HF)混合,并借助于微波加压消化而消化。接下来,将溶解的样品转移到试管中,并用超纯水将其封顶。将测量溶液泵送到测量仪器中,在其中将其雾化,并且将气雾剂引入氩等离子体中,其中对样品的成分进行汽化、雾化、激发和部分电离。然后检测当原子/离子返回到基态时所发射的光。发射光的波长是包含在样品中的相应元素的特征。波长的强度与相应元素的浓度成比例。
根据本发明的粉末的第一粒子级分优选粒度d50为10nm至1000nm。第二粒子级分优选粒度d50为0.5μm至50μm。优选通过激光衍射确定粒径。
在特别优选的具体实施例中,粉末包括粒度d50为30μm至120μm的第三粒子级分。
因此,用于生产多孔材料的根据本发明的粉末的金属氧化物粉末的粒径d50可为0.001μm至120μm。
粒子级分可以一定的混合比率:
第一粒子级分:5-20重量%
第二粒子级分:40-70重量%
第三粒子级分:10-40重量%
由于此一混合比率,特别是由于使用具有纳米级粒子的粒子级分,通过使用根据本发明的粉末,在甚至低温下的多孔材料生产中可以获得良好的烧结结果。关于粒径分布,使用根据DIN EN 725-5标准的测量方法。对于大小范围为1μm至100μm的粒子的测量,使用来自新帕泰克(Sympatec)的激光衍射装置(Helos 0724)。使用来自堀场(Horiba)公司的激光衍射装置(LA-950)测量大小范围小于1μm的粒子。
用于生产多孔材料的根据本发明的粉末也可用于生产矿物绝缘导体和/或用于生产矿物绝缘线。
本发明的另一独立方面涉及一种生产多孔材料的方法,特别是一种生产根据本发明的多孔材料的方法。
根据本发明的方法的特征在于以下方法步骤:
a)特别地由根据本发明的粉末和溶剂(特别是无机溶剂,尤其优选水)制备包含金属氧化物粉末的粉末的分散液;
b)提供模具或载体;
c)用所述分散液填充所述模具或用所述分散液涂覆所述载体。
分散液有可能包含额外的组分,例如添加剂和/或泡沫抑制剂和/或助流剂和/或稳定剂。
根据本发明的方法可以另外包括以下步骤:
d)加热填充的模具/涂覆的载体,并且然后
e)冷却填充的模具/涂覆的载体和任选地
f)移除模具/载体。
步骤c),特别是填充模具,可以在降低的压力下进行。
如果要为组件提供涂层和/或将其包埋于铸造化合物中,则这一组件应首先至少暂时地固定在模具中//粘附在那里。组件固定在步骤b)中进行。
特别是在步骤f)之后,即在模具和/或载体已被移除之后,在另一加工步骤中,多孔材料可以被研磨和/或抛光和/或钻孔和/或铣削和/或熔接和/或焊接。
分散液的固体含量优选合计为70重量%至90重量%。分散液的固体含量尤其优选合计为85重量%。固体含量可以简单的称重方法来确定。
另外,分散液的粘度可以达到5Pa·s至15Pa·s。分散液的粘度优选根据DIN53019标准使用Brookfield DV3T流变仪来确定。
在步骤d)中,优选将模具/涂覆的载体加热至100℃至1400℃、尤其是400℃至1100℃、特别是600℃至900℃的温度。
步骤c)与e)之间的体积收缩率优选达到小于5%。在本发明的特别优选的具体实施例中,步骤c)与e)之间的体积收缩率达到小于4%。
在步骤c)与e)之间,特别是在充分加热下,如下进行多孔材料(特别是铸造化合物)的体积收缩率的测量:
1.用分散液填充试管。
2.在填充后确定分散液的填充水平(h1)。
3.将试管中的分散液在室温下干燥至少48小时,并且然后从试管中移出。
4.在600℃至900℃的温度下加热生坯。
5.在加热之后确定固体的高度(h2)。
加热下的体积收缩率(DV)的等式为:DV=(h1-h2)/h1·100%。
模具和/或载体可由例如金属和/或金属合金和/或陶瓷和/或玻璃陶瓷和/或木材和/或纸和/或聚合物和/或塑料制成。模具可以另外设计成管或套管或盒子或球或半球。
然而,载体可设计成膜或薄片或衬底或层。
在本发明的一个具体实施例中,模具可以是消失铸造模(lost casting mold)。另外,可以在步骤c)之后,特别是在干燥过程之后按照预定移除模具,然而,所述干燥过程与根据步骤d)的加热步骤无关。
在根据本发明的方法的范围内,在步骤b)中,有可能将待包覆和/或包埋的组件,特别是电气组件和/或电子组件和/或线材和/或管和/或传感器,特别是铂传感器和/或连接件和/或套管和/或单线或多线同轴电缆布置在模具中或载体上。
结合根据本发明的生产多孔材料的方法,实现了与已结合多孔材料和/或根据本发明的用于生产多孔材料的粉末所描述的优点类似的优点。
本发明的另一独立方面涉及具有涂层的组件和/或包埋于铸造化合物中的组件,其中一或多个涂层和/或铸造组件是根据本发明的多孔材料和/或根据本发明生产的多孔材料。
所述组件可以是传感器,特别是温度传感器。所述组件优选地安装在机动车的排气管线和/或发动机***中。所述部件也可以是线材和/或管和/或连接件和/或套管和/或单线同轴电缆//单芯和/或多线//芯同轴电缆。
根据本发明的组件,特别是根据本发明的传感器可以承受以下应力中的至少一种,优选几种:
a)在25℃与1100℃之间的至少30,000次热冲击循环,至少1000K/s的温度梯度;
b)在1100℃下储存至少1000小时;
c)在最大5kHz振动频率的滑动正弦下进行至少150小时的热振动器测试;
d)在室温下进行10次摆锤冲击测试,其中加速度为至少8000g。
下面基于一个示例性实施例对本发明进行更详细的说明。
包埋于铸造化合物中的铂传感器通过根据本发明的方法来生产。
为此,首先,由高纯度氧化铝(Al2O3)粉末和水制备分散液。氧化铝粉末的纯度为至少99.99%。氧化铝粉末具有三个粒子级分,第一粒子级分的粒度d50为100nm,第二粒子级分的粒度d50为1μm,并且第三粒子级分的粒度d50为70μm。
首先,将铂传感器定位在保护套管中并固定在那里。在下一步骤中,将已描述的粉末倒入保护套管中。
然后加热填充的保护套管。分散液的固体含量为85%。在600℃至900℃的温度下加热其内部具有铂传感器和分散液的保护套管。
在加热之后,将其中具有传感器和然后存在的铸造化合物和/或多孔材料的一或多个保护套管冷却。在用分散液和多孔材料和/或最后生产的铸造复合物填充的保护套管之间的体积收缩率为4%。
在生产包埋于铸造化合物中的传感器之后,所得铸造化合物在1000℃的温度下的比电阻为2.0·106Ω·cm。比电阻可以通过伏安检测法来确定。
多孔材料和/或铸造化合物的孔隙率为35%。铸造化合物的孔体积为0.14cm3/g。孔径d50在78与98nm之间。孔隙率、孔体积和孔径d50通过汞孔隙率测定法来确定。
铸造化合物的热膨胀系数达到6.5至8.5·10-6/K。热膨胀通过膨胀测定法来确定。然而,3点弯曲强度量为46N/mm2。因此,这是一种满足耐腐蚀性、耐热冲击性和耐振动性所有要求的铸造化合物。
此外,甚至在高达1100℃的高温下,铸造化合物仍具有电绝缘效果。由于为铂传感器所选的氧化铝粉末,铂传感器遭受较低的中毒。
Claims (19)
1.一种多孔材料,特别是传感器用铸造化合物,
其特征在于
在1000℃的温度下,比电阻为至少105Ω·cm,特别是至少106Ω·cm。
2.根据权利要求1所述的多孔材料,
其特征在于
这种金属氧化物特别包括氧化铝(Al2O3)和/或氧化镁(MgO)和/或氧化铍(BeO)。
3.根据权利要求1或2所述的多孔材料,
其特征在于
这种材料含有高纯度氧化铝(Al2O3),特别是由高纯度氧化铝(Al2O3)组成,其中所述氧化铝(Al2O3)的纯度达到至少99.99%。
4.根据权利要求1至3所述的多孔材料,
其特征在于
以所述多孔材料的总重量计,所述多孔材料的碳C含量小于1000ppm,特别是小于500ppm,特别是小于250ppm,特别是小于100ppm。
5.根据前述权利要求中任一权利要求所述的多孔材料,
其特征在于
所述材料的孔隙率D达到25%至50%和/或孔体积达到0.05cm3/g至0.5cm3/g,其中所述孔隙率和/或所述孔体积通过汞孔隙率测定法来确定。
6.根据前述权利要求中任一权利要求所述的多孔材料,
其特征在于
孔径d50为50至150nm。
7.一种用于生产多孔材料、特别是根据权利要求1至6中任一权利要求所述的多孔材料的粉末,其包括金属氧化物粒子,特别是氧化铝粒子(Al2O3)和/或氧化镁粒子(MgO)和/或氧化铍粒子(BeO),
其特征在于
所述粉末具有至少两个粒子级分,特别是至少三个粒子级分,其中各别粒子级分的粒度d50具有不同值。
8.根据权利要求7所述的粉末,
其特征在于
第一粒子级分的粒度d50为10nm至1000nm且第二粒子级分的粒度d50为0.5μm至50μm。
9.根据权利要求8所述的粉末,
其特征在于
第三粒子级分的粒度d50为30μm至120μm。
10.根据权利要求7至9中任一权利要求所述的粉末,
其特征在于
所述金属氧化物粒子的粒径d50为0.001μm至120μm。
11.一种生产多孔材料、特别是根据权利要求1至6中任一权利要求所述的多孔材料的方法,
其特征在于以下方法步骤:
a)制备包括金属氧化物粒子的粉末、特别是根据权利要求7至10中任一权利要求所述的粉末,和溶剂、特别是无机溶剂、尤其优选水的分散液;
b)供应模具或载体;
c)用所述分散液填充所述模具或用所述分散液涂覆所述载体。
12.根据权利要求11所述的方法,
其特征在于
额外步骤:
d)加热经填充的所述模具/经涂覆的所述载体,并且然后
e)冷却所述填充的模具/所述涂覆的载体和任选地
f)移除所述模具/所述载体。
13.根据权利要求11或12所述的方法,
其特征在于
所述步骤c)、特别是填充所述模具是在在降低的压力下进行。
14.根据权利要求11至13中任一权利要求所述的方法,
其特征在于
所述分散液的固体含量达到70重量%至90重量%和/或所述分散液的粘度达到5Pa·s至15Pa·s。
15.根据权利要求12至14中任一权利要求所述的方法,
其特征在于
在步骤d)中,将所述模具/涂覆的载体加热至100℃至1400℃、特别是400℃至1100℃、特别是600℃至900℃的温度。
16.根据权利要求12至15中任一权利要求所述的方法,
其特征在于
步骤c)与e)之间的体积收缩率达到小于5%。
17.根据权利要求11至15中任一权利要求所述的方法,
其特征在于
在步骤b)中,将待包覆和/或包埋的组件,特别是电气组件和/或电子组件和/或线材和/或管和/或传感器和/或连接件和/或套管和/或具有一或多个线//芯的同轴电缆布置在所述模具中或所述载体上。
18.一种具有涂层和/或包埋于铸造化合物中的组件,其中所述涂层和/或所述铸造化合物是根据权利要求1至6中任一权利要求所述的多孔材料和/或根据权利要求11至17中任一权利要求生产的多孔材料。
19.根据权利要求18所述的组件,
其特征在于
其是传感器,特别是温度传感器且优选是安装在机动车的排气管线和/或发动机***中。
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DE102016115183.1A DE102016115183A1 (de) | 2016-08-16 | 2016-08-16 | Poröses Material, Pulver zur Herstellung eines porösen Materials, Verfahren zur Herstellung eines porösen Materials und Bauteil |
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PCT/EP2017/070714 WO2018033553A1 (de) | 2016-08-16 | 2017-08-16 | Poröses material, pulver zur herstellung eines porösen materials, verfahren zur herstellung eines porösen materials und bauteil |
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CN116514575A (zh) * | 2023-05-05 | 2023-08-01 | 郑州大学 | 一种氧化铍电极材料、铍-氧化铍金属陶瓷及其制备方法 |
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CN109641800B (zh) | 2022-06-21 |
KR102227277B1 (ko) | 2021-03-11 |
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