CN106029607B - 由用于3-d加强的氧化物/氧化物复合物材料制造的部件以及制造其的方法 - Google Patents

由用于3-d加强的氧化物/氧化物复合物材料制造的部件以及制造其的方法 Download PDF

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CN106029607B
CN106029607B CN201580008763.3A CN201580008763A CN106029607B CN 106029607 B CN106029607 B CN 106029607B CN 201580008763 A CN201580008763 A CN 201580008763A CN 106029607 B CN106029607 B CN 106029607B
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yarns
fiber
oxide
texture
warp
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CN106029607A (zh
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帕斯卡尔·迪斯
埃里克·布伦
埃里克·拉维斯瑞
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Hai Ruikelizi
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Abstract

一种由包括纤维加强(310)的氧化物/氧化物复合材料制造的部件(300)，该纤维加强包括通过三维编织联结在一起的多层经线(312)和纬线(311)，用耐火氧化物(320)的基质填充加强线之间的空间。该部件的特征在于纤维加强具有选自下列编织法之一的织物编织：联锁、多层、多缎纹和多斜纹，并且经纱和纬纱中的线数是40和20根线/cm之间。纤维加强还具有40％和51％之间的纤维体积密度。

Description

由用于3-D加强的氧化物/氧化物复合物材料制造的部件以及 制造其的方法
背景技术
本发明涉及制造由氧化物/氧化物类型的复合材料所制造的部件的方法，即，该复合物材料包括由耐火氧化物纤维制造的纤维加强，该纤维加强被同样地由耐火氧化物制造的基质致密。
大部分氧化物/氧化物复合材料部件通过下面两种方式制备：
·通过堆叠二维层编织的氧化物纤维织物制造纤维织构，以及用含有氧化物填料的悬浮液浸渍织构，填充的预制件然后经受烧结；或者
·通过缠绕之前已经被浸入在含有氧化物填料的悬浮液中的氧化物纤维纱线来制造纤维织构，填充的预制件然后经受烧结。
然而，通过这些制备方法所获得的氧化物/氧化物复合材料的机械特征在一些方向上保持了有限性。特别地，这些材料具有低剪切强度。
通过在连续的经纱和纬纱之间三维编织制造所获得的纤维织构能够使得材料的机械强度被增强。在这种情况下，可以引起填充的悬浮液穿入到纤维织构中，该纤维织构可以具有达到几十毫米的厚度，这仅取决于通过利用压力梯度方法的意欲应用，该方法是诸如称为树脂传递模成型(RTM)的注射成型类型的方法，或者亚微米粉末吸入法(SPS)。
氧化物/氧化物复合物材料中纤维的体积分数是将要考虑用于获得材料的最终机械特征的基础参数之一。这就是为什么当制备氧化物/氧化物复合材料时，需要使用特定的工艺装备压缩纤维织构。在工艺装备中的干燥步骤期间，基质中网络形式的裂纹存在于纱线之间。网络裂纹导致脱膜期间浸渍的预制件膨胀，因此导致最终阶段中材料机械特性的大大降低。
一种补救膨胀的已知方法包括添加有机粘合剂，例如聚乙酸乙烯酯(PVA)到最初的悬浮液中，因此有助于预制件已经干燥后系统的粘合，防止上述膨胀现象。
为了在单个浸渍步骤中获得高机械特性，必须使用具有足够体积百分比填料的崩料。在这种情况下，添加有机粘合剂改变了崩料的特性。它的特性从是牛顿特性(独立于流速的粘性)改变到剪切稀化特性(依赖于流速的粘性)。当使用通过SPS技术制备时，这种现象导致在材料内组份中的不均匀外观。
更精确地，考虑材料作为整体时，对纤维织构内悬浮液流动的差控制导致跨越材料厚度的组份梯度(纤维/基质比率)的外观。一旦通过烧结已经稳定了填料，材料内更局部地不受控制的尺寸和分布的孔就会形成。
发明内容
本发明的目的是补救上述缺陷，并且提出一种方案，该方案可以在单个浸渍步骤中具有由使用SPS技术所制备的氧化物/氧化物复合材料制造的部件，不需要使用附加的有机粘合剂，该部件包括通过三维编织所获得的加强以及具有相对于现有技术部件改进的机械特性。
为此，本发明提出了一种由包括纤维加强的氧化物/氧化物复合材料所制造的部件，该纤维加强由通过三维编织互连的多个经纱层和纬纱层构成，同时用耐火氧化物基质填充加强纱线之间具有的空间；
部件的特征在于纤维加强具有选自下列编织法的编织法：联锁；多平纹；多缎纹；多斜纹；并且经线和纬线数范围是每厘米4根纱线(纱线/cm)到20根纱线/cm，并且其特征在于纤维加强具有范围在40％到51％的纤维体积分数。
关于具有上述特征的纤维加强，并且考虑调整对选定织构变体的纤维体积分数，加强的纱线之间存在的空间具有小于5倍的纤维加强的纱线的最大部分的维度。通过以这种方式限制纱线之间存在的空间的尺寸，限制了材料中存在的基质块的尺寸，以致于每个基质块不具有大于5倍的加强纤维的最大部分的任何维度。通过以这种方式限制氧化物/氧化物材料中基质块的尺寸，已经观察到了特性，可以防止裂纹出现在其中。因此，氧化物/氧化物复合材料部件具有改进的机械特性。
在本发明部件的特定方面，在单调牵引中，在室温以及在经线方向上，它具有：
·范围在120G帕斯卡(GPa)到170GPa的弹性模数；
·不小于0.35％的破裂变形；以及
·大于250兆帕斯卡(MPa)的破裂应力；
纤维加强的纱线可以由一种或多种下列材料所构成的纤维制造：氧化铝；莫来石；硅石；硅酸铝；和硅酸硼。
基质的材料可以选自：氧化铝；莫来石；硅石；硅酸铝；和磷酸铝。基质可选地可以掺杂有一种或多种材料，用于给部件的最终材料增加特定的功能。
本发明也提供了一种制造氧化物/氧化物复合材料部件的方法，该方法包括下列步骤：
·通过耐火氧化物纱线的三维编织形成纤维织构；
·压缩纤维织构；
·在纤维织构的一侧上放置崩料，该崩料包含耐火氧化物颗粒的亚微米粉末；
·建立压力差以迫使崩料通过纤维织构；
·过滤已经通过纤维织构的崩料的液体，以保留耐火氧化物颗粒的粉末在所述织构内部；
·干燥填充的预制件；和
·烧结耐火氧化物颗粒的亚微米粉末，以在预制件中形成耐火氧化物基质；
该方法的特征在于在形成纤维织构的步骤期间，用选自下面编织法的编织法编织纱线：联锁；多平纹；多缎纹和多斜纹；同时经线和纬线数范围在4根纱线/cm到20根纱线/cm，并且其中在压缩步骤后，所述纤维加强具有范围在40％到51％的纤维体积分数。
这产生了具有3D编织加强的氧化物/氧化物复合材料部件，该部件在遍布它们的体积上是完全均匀的，并且不包括可能降低部件的机械特性的裂纹或孔。
预制件的纱线可以是由一种或多种下列材料所构成的纤维制造的纱线：氧化铝；莫来石；硅石；硅酸铝；和硅酸硼。
亚微米颗粒可以由选自下列的材料制造：氧化铝；莫来石；硅石；硅酸铝；和磷酸铝；可选地带有附加的填料，用于给部件的材料增加功能。
附图说明
从参考附图作为非限制性实施例所给出的本发明的特定实施方式的下面描述，可以显现本发明的其它特征和优点，其中：
图1表示根据本发明的纤维织构的实施方式，三维联锁编织的平面。
图2表示根据本发明的纤维织构的实施方式，三维多平纹编织的平面。
图3表示根据本发明的纤维织构的实施方式，三维多缎纹编织的平面。
图4表示根据本发明的纤维织构的实施方式，三维多斜纹编织的平面。
图5是一种示意图，表示通过SPS技术，用耐火氧化物颗粒渗透纤维织构。
图6是如现有技术所制造的由氧化物/氧化物类型材料所制造的部件的剖面的显微图。
图7A、7B和7C是根据本发明由氧化物/氧化物复合材料所制造的部件的显微图。以及
图8是表示用于本发明的纤维织构的设计域的图。
具体实施方式
制造根据本发明的由氧化物/氧化物复合材料制成的部件的方法开始于制造纤维织构，该纤维织构将要用于形成部件的加强。
根据本发明，通过多个经纱和多个纬纱之间的三维编织制造纤维织构，使用对应于选自下列编织法之一的编织法，经纱层与纬纱互连：互锁；多平纹；多缎纹；和多斜纹；并且经线和纬线数范围在4根纱线/cm到20根纱线/cm，通过这种方法所获得的织构然后被压缩以具有范围在40％到51％的纤维体积分数，纤维织构中每个纱线或纤维都具有400个长丝到700个长丝的长丝数量。图8表示根据本发明的用于纤维织构的设计域D，该域D限定了涉及本发明纤维织构的参数需要被呈现的数值。
纤维织构的这些特征可以确保在纱线之间不存在具有大于5倍的纱线的最大部分的维度的空间。因此，一旦基质已经形成在织构内，织构纱线之间存在的基质块具有所有都小于5倍的纱线的最大部分的维度，因此可以防止裂纹出现在部件的最终材料中。
术语“基质块”用于在这里意指位于两个或多个纱线之间的基质的任何连续部分。使用术语“基质块的维度”在此指基质块的任何长度、宽度、深度、厚度、高度或实际上直径，并且还是更通常方式指在直线方向上可以测量的任何尺寸。
术语“线数”用在此处指在经纱方向上或在纬纱方向上每单位长度的纱线数量。
术语“三维编织”和“3D编织”用在这里指一种编织技术，其中至少一些经纱互连多个纬纱层上的纬纱。
在整个下面的描述中，并且在所有图中，为了习惯和方便的原因表述和表示经纱从它们的路径被偏转，以控制住一层或多层纬纱中的纬纱。然而，可以为了经纱和纬纱之间互换的作用，这也必须被考虑为权利要求所保护的范围。
术语“互锁编织或织物”用在这里意指3D编织，其中每层经纱互连多层纬纱，同时在相同经纱列中的所有纱线在编织平面中具有相同的运动。图1是互锁编织法的8个平面的图示，具有7层经纱C1和8层CT1纬纱T1。在所示的互锁编织中，经纱T1的层CT1由在经纱方向上彼此偏移的两个相邻的半层ct1组成。因此，在交错构造中具有16个半层的纬纱。每个经纱C1互连3个半层的纬纱。采用不交错的纬纱布置也是可以的，两个相邻层纬纱中的纬纱在相同列中被对齐。
举例说明，如图1中所示，使用联锁编织法，通过3D编织可以制造本发明的纤维织构，具有8根纱线/cm，10根纱线/cm和12根纱线/cm的经线和纬线数，或者12根纱线/cm的经线数和5根纱线/cm的纬线数。
术语“多平纹编织法或织物”用在这里意指具有多个纬纱层的3D编织法，其中每层的基础编织等同于常规的平纹类型编织，但是具有互连纬纱层的一些编织的交叉点。图2表示多平织织物的平面，其中在与纬纱层CT2相关的常规2D平面编织中经纱C2偶尔地从它们的路径转向，以控制住相邻层的纬纱T2，因此形成互连两个相邻纬纱层的特定的平交叉点PT。在特定的平交叉点PT，经纱C2通过位于两个相邻纬纱层CT2中相同列中两个纬纱T2周围。
举例说明，如图2所示，使用多平纹编织法，通过3D编织可以制造本发明的纤维织构，并且具有20根纱线/cm的经线和纬线数。
术语“多缎纹编织法或织物”用在这里意指具有多个纬纱层的3D编织法，其中每层的基础编织等同于常规的缎纹类型编织，但是具有互连纬纱层的一些编织的交叉点。图3表示多缎织织物的平面，其中，除了位于织构表面的经纱以外的每个经纱C3在一个方向上和在另一个方向上被交替地转向，以控制住第一纬纱层CT3中n个纬纱中的一个纬纱T3以及与第一纬纱层相邻的第二纬纱层CT3中n个纬纱中的一个纬纱T3，其中n是大于2的整数，因此互连两个层。
举例说明，如图3所示，使用多缎纹编织法，通过3D编织可以制造本发明的纤维织构，并且具有10根纱线/cm的经线和纬线数。
术语“多斜纹编织法或织物”用在这里意指具有多个纬纱层的3D编织法，其中每层的基础编织等同于常规的斜纹类型编织，但是具有互连纬纱层的一些编织的交叉点。图4表示多斜纹织物的平面，其中，除了位于织构表面的经纱以外的每个经纱C4被转向，以控制住纬纱层CT4中或多个相邻纬纱层CT4中成对的纬纱T4。
举例说明，如图4所示，使用多斜纹编织法，通过3D编织可以制造本发明的纤维织构，并且具有8根纱线/cm的经线和纬线数。
用于编织纤维织构的纱线特别地可以由任何一种下列材料所构成的纤维制造，该纤维织构将要形成氧化物/氧化物复合材料部件的纤维加强：氧化铝；莫来石；硅石；硅酸铝；硅酸硼；或者多种这些材料的混合物。
一旦已经制造纤维织构，就压缩它以调整其纤维体积含量达到范围在40％到51％的数值。使用工艺装备100进行压缩，该工艺装备100用于在纤维织构内沉积耐火氧化物颗粒，如下面所详述。通过栅格140压缩织构10，穿孔该栅格140以使崩料通过，在随后操作期间使用该崩料。在工艺设备100中对应于期望应用于织构的压缩厚度Ec的位置，通过保持设备，例如通过螺钉(图5中未示)，栅格140保持压靠于纤维织构。当脱膜后(即，通过SPS技术浸渍织构，然后干燥它后)没有纤维织构的膨胀时，部件的最终厚度等于压缩厚度Ec。
纤维体积分数对应于由所制造织构的总体积内纤维所占据的织构总体积的分数。举例说明，具有平面板形状的纤维织构，使用下面参数计算纤维体积分数：
·织构的长度L；
·织构的宽度l；
·织构的厚度e；
·纤维的密度d；和
·织构每单位面积的重量Ms。
具体地，纤维体积分数Tvf等于纤维体积Vf除以织构的总体积。所用的纤维体积Vf等于所用的纤维重量，即，Ms.L.l，除以纤维密度d，即：Vf＝Ms.L.l/d。
因为板形式的纤维结构的总体积等于L.l.e，使用下面公式计算纤维体积分数
Tvf：Tvf＝Ms/(e.d) (1)
因此，当期望获得具有范围在40％到51％数值的纤维体积分数的纤维织构时，调整纤维织构的压缩厚度，这样在压缩后，它具有可以获得范围在40％到51％的纤维体积分数的厚度e，根据公式(1)所规定的，根据织构的每单位面积的重量Ms和纤维密度确定压缩厚度。
然后，使用亚微米粉末吸入法(SPS)的已知技术，耐火氧化物颗粒沉积在纤维织构内。为此，并且如图5中所示，使用上述3D编织法之一所制造的纤维织构10被放置在工艺装备100的外壳110中。过滤器120提前插入在外壳110的底部111和纤维织构10之间，底部111包括开口1110。放置织构10在外壳110中之后，用于在织构中形成耐火氧化物基质的崩料130沉积在纤维织构10的顶部面上，即，与面对过滤器120的其面相对的织构的面。崩料130对应于含有耐火氧化物颗粒的亚微米粉末的悬浮液。举例说明，崩料130可以对应于由氧化铝粉末构成的含水悬浮液，具有范围在27％到42％的体积分数，该氧化铝粉末具有范围在0.1微米(μm)到0.3μm的平均颗粒大小(D50)，用硝酸(pH范围在1.5到4)酸化悬浮液。除了氧化铝外，构成亚微米粉末的耐火氧化物颗粒同样地可以很好地由选自莫来石、硅石、硅酸铝和磷酸铝的材料制造。耐火氧化物颗粒也可以与锆、稀土氧化物或者能够增加最终材料特定功能的任何其它填料的颗粒(炭黑、石墨、碳化硅等)混合。
用盖子112关闭外壳110后，通过管道1120，将由压缩空气或氮气组成的气流F1引入到外壳110中。气流F1用于施加压力P1，该压力P1迫使崩料130穿透到织构10中。与插入气流F1联合，例如，使用初级真空泵(图5中未示出)从外壳110底部111的外侧，通过开口1110进行泵吸P，以迫使崩料130迁移通过织构10。校准过滤器120以保留崩料中存在的耐火氧化物颗粒，同时崩料的液体通过开口1110排出。因此，耐火氧化物颗粒通过沉积作用变得逐渐地沉积在织构中。
这产生了填充有耐火氧化物颗粒，在该实施例中，上述类型的氧化铝颗粒的纤维预制件。然后在35℃和95℃范围的温度干燥预制件，随后预制件在1000℃和1200℃范围的温度的空气下经受烧结热处理，以一起烧结耐火氧化物颗粒，因此在预制件中形成耐火氧化物基质。这产生了由氧化物/氧化物复合材料制造的部件，具有通过3D编织所获得的纤维加强，不包括加强纱线之间存在的基质块中的裂纹。
图6是由现有技术氧化物/氧化物复合材料，特别地在该实施例中由氧化铝基质致密的氧化铝纤维加强制造的部件200的剖面的显微图，其纤维加强210由纬纱层211和经纱层212之间3D编织形成，具有互锁编织，8根纱线/cm的经线和纬线数，以及具有38％的纤维体积分数。以与上述方式相同的方式即，通过SPS技术，接着是填充预制件的干燥和烧结制造部件200。如图6中可以看到的，纤维加强210所限定的编织和线数导致在材料中形成基质220块221，该基质块在至少一个方向上具有维度，该维度大于5倍的加强纱线的最大部分，在该实施例中纬纱211的部分。如图6中可以看到的，因为没有限制基质块的尺寸小于5倍的最大部分，在材料中已经形成裂纹230，它们中的一些甚至已经通过加强纱线，显著地降低了部件200的机械特性。
图7A、7B和7C是分别地在部件300、400和500的经纱方向上(显微图的长度方向对应于经纱方向，并且显微图的高度方向对应于z方向)剖面的显微图，每个部件由本发明的氧化物/氧化物复合材料，即，在本实施例中由氧化铝基质所致密的氧化铝纤维加强所制造。
在图7A中，使用具有10根纱线/cm的经线和纬线数和43.4％的纤维体积分数的多缎纹编织法，通过纬纱线层311和经纱线层312之间的3D编织形成该实施例中部件300的纤维加强310。
在图7B中，使用具有12根纱线/cm的经线数，5根纱线/cm的纬线数和44.8％的纤维体积分数的联锁编织法，通过纬纱线层411和经纱线层412之间的3D编织形成该实施例中部件400的纤维加强410。
在图7C中，使用具有12根纱线/cm的经线和纬线数和43.5％的纤维体积分数的联锁编织法，通过纬纱线层511和经纱线层512之间的3D编织形成该实施例中部件500的纤维加强510。
以与上述方式相同的方式即，通过SPS技术，接着是填充预制件的干燥和烧结制造部件300、400和500。
所限定用于纤维加强310、410和510的编织法、线数和纤维体积分数分别地导致在材料中形成基质320、420和520的块321、421和521，该基质块在所有方向上都具有小于5倍的加强纱线最大部分的维度。如图7A、7B和7C中可以看到的，因为限制基质块尺寸小于5倍的加强纱线的最大部分，在材料中不存在裂纹。因此，部件300、400和500具有比部件200更优越的机械特性。
下面的表给出了根据图6、7A、7B和7C部件的每单位面积重量Ms、板厚度e、密度d(氧化铝纤维)和纤维体积分数所获得的数值。
部件 织构 Ms(g/m<sub>2</sub>) e(mm) d TVf
部件200(图6) 8/8联锁 6667 4.5 3.9 38
部件300(图7A) 10/10多缎织 5420 3.2 3.9 43.4
部件400(图7B) 12/5联锁 5420 3.1 3.9 44.8
部件500(图7C) 12/12联锁 5770 3.4 3.9 43.5
可以看出图6的部件200是具有纤维体积分数不位于40％到51％范围的仅有的部件。也可以看出部件200是在其材料中由于基质块存在而具有裂纹的仅有部件，该基质块在至少一个方向上具有大于5倍的加强纱线的最大部分的维度。
本发明的方法能够使用SPS技术以及从三维编织纤维织构制造氧化物/氧化物复合材料部件，该部件在遍布它们的体积上是完全地均匀的，没有裂纹或孔。根据本发明的这些部件具有在单调牵引中、在室温和在经线方向上测量的下列机械特性：
·范围在120GPa到170GPa的弹性模数；
·不小于0.35％的破裂变形；以及
·大于250MPa的破裂应力。
尽管本发明部件的氧化物/氧化物材料的3D编织纤维加强纱线可以被包括在中间阶段中，但是本发明的方法可以制造具有3D编织纤维加强的氧化物/氧化物复合部件，没有纱线的中间阶段，并且自然地在材料中没有裂纹。

Claims (7)

1.一种由包括纤维加强的氧化物/氧化物复合材料所制造的部件，该纤维加强由通过三维编织互连的多个经纱层和纬纱层构成，同时用耐火氧化物基质填充加强纱线之间具有的空间；
其中纤维加强具有选自下列编织法中一种或多种的编织法：联锁；多平纹；多缎纹；多斜纹；并且经线和纬线数范围是4根纱线/cm到20根纱线/cm，并且纤维加强具有范围在40％到51％的纤维体积分数，使得加强的纱线之间存在的空间具有小于5倍的纤维加强的纱线的最大部分的维度。
2.根据权利要求1所述的部件，其中在单调牵引中、在室温以及在经线方向上，它具有：
·范围在120GPa到170GPa的弹性模数；
·不小于0.35％的破裂变形；以及
·大于250MPa的破裂应力。
3.根据权利要求1所述的部件，其中纤维加强的纱线由一种或多种下列材料所构成的纤维制造：氧化铝；莫来石；硅石；硅酸铝；和硅酸硼。
4.根据权利要求1所述的部件，其中基质材料选自下列材料中的一种或多种：氧化铝；莫来石；硅石；硅酸铝；和磷酸铝。
5.一种制造氧化物/氧化物复合材料部件的方法，该方法包括下列步骤：
·通过耐火氧化物纱线的三维编织形成纤维织构；
·压缩所述纤维织构；
·在纤维织构的一侧上放置崩料，该崩料包含耐火氧化物颗粒的亚微米粉末；
·建立压力差以迫使崩料通过纤维织构；
·过滤已经通过纤维织构的崩料的液体，以保留耐火氧化物颗粒的粉末在所述织构内部；
·干燥填充的预制件；和
·烧结耐火氧化物颗粒的亚微米粉末，以在预制件中形成耐火氧化物基质；
其中在形成纤维织构的步骤期间，用选自下面编织法中一种或多种的编织法编织纱线：联锁；多平纹；多缎纹和多斜纹；同时经线和纬线数范围在4根纱线/cm到20根纱线/cm，并且其中在压缩步骤后，所述纤维加强具有范围在40％到51％的纤维体积分数，使得加强的纱线之间存在的空间具有小于5倍的纤维加强的纱线的最大部分的维度。
6.根据权利要求5所述的方法，其中预制件的纱线由一种或多种下列材料构成的纤维制造的：氧化铝；莫来石；硅石；硅酸铝；和硅酸硼。
7.根据权利要求5所述的方法，其中亚微米粉末由选自下列的材料中的一种或多种材料制造：氧化铝；莫来石；硅石；硅酸铝；和磷酸铝。
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