CN107074668A - 陶瓷基复合材料的制造方法 - Google Patents
陶瓷基复合材料的制造方法 Download PDFInfo
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Abstract
一种陶瓷基复合材料的制造方法,包括:将含有SiC粉末的骨料粉末、与含有选自由热塑性树脂和蜡所组成的组中的一种以上粘合剂混炼以得到由骨料粉末和粘合剂构成的组合物,对组合物施压以制成片,使由含SiC纤维的增强纤维构成的织物与片交替地层叠,施压织物与片的层叠体,生成使增强纤维相互结合的基质。
Description
技术领域
本公开内容涉及能够适用于飞机用喷气发动机等要求高温强度的仪器的陶瓷基复合材料的制造方法。
背景技术
陶瓷具有极高的耐热性,但是另一方面,大多数陶瓷存在脆这样的缺点。一直以来,为了克服脆性,尝试了将陶瓷作为母材(基质)、与SiC等无机物的纤维进行复合化。
为了进行复合化,提出了气相浸渍(CVI)、液相浸渍(例如聚合物熔融浸渍热分解(PIP))、固相浸渍(SPI)、熔融金属浸渍(MI)等方法。例如根据PIP法,对由SiC等纤维形成的织物进行聚合物溶液浸渍,将其在高温烧成而发生陶瓷化,从而该陶瓷成为基质而与纤维进行复合化。聚合物溶液可以根据想要生成的陶瓷而适当选择,例如制成含有聚碳硅烷的溶液的话,则产生由SiC形成的基质。
还提出了将这些方法组合而得到的技术。专利文献1公开了相关的技术。
现有技术文献
专利文献
专利文献1:日本特开2008-081379号公报
发明内容
发明所要解决的问题
如果纤维间残留有孔隙,当然对陶瓷基复合材料的强度、韧性不利。此外,如果高温的空气、水蒸气通过该孔隙侵入陶瓷基复合材料,则由氧化引起的劣化会发展。然而,通过上述任意的方法,都不能容易地利用基质完全堵塞纤维间的孔隙。因此,反复进行浸渍变得非常耗工。由于在每次浸渍中反复进行干燥和烧成,最终制品的制造需要1个月以上。
将孔隙从陶瓷基复合材料消除到何种程度、此外如何有效地堵塞孔隙,这是该技术领域长期存在的技术课题。
用于解决课题的方法
根据一个方面,陶瓷基复合材料的制造方法包括:将含有陶瓷的骨料粉末、与含有选自由热塑性树脂和蜡所组成的组中的一种以上粘合剂混炼,以得到由上述骨料粉末和上述粘合剂构成的组合物,对上述组合物施压以制成片,将由含陶瓷的增强纤维构成的织物与上述片交替地层叠,施压上述织物与上述片的层叠体,生成使上述增强纤维相互结合的基质。
发明效果
在纤维间的孔隙使骨料粉末有效地浸渍,由此能够有效地堵塞该孔隙。
附图说明
图1为概括地说明一个实施方式的陶瓷基复合材料的制造方法的流程图。
图2A为示意性表示制造方法中的混炼工序的图。
图2B为示意性表示制造方法中的片化工序的图。
图3A为示出增强纤维织物与含陶瓷片的层叠体的示意性截面图,为施压前的状态的图。
图3B为示出增强纤维织物与含陶瓷片的层叠体的示意性截面图,为被施压后的状态的图。
图4A为成形体的例示性立体图。
图4B为最终制品的例示性立体图。
具体实施方式
以下,参照附图说明若干实施方式。
一个实施方式的陶瓷基复合材料的适当用途为飞机用喷气发动机的构成部件那样的暴露于高温环境的机械部件,可例示出涡轮叶片、燃烧室、加力燃烧室等。当然也可以适用于其他用途。
一个实施方式的陶瓷基复合材料大体具备:由碳化硅(SiC)那样的无机物纤维形成的织物、以及使由SiC那样的无机物形成的上述织物结合的基质。该陶瓷基复合材料的制造方法大体包括:使作为基质原料的骨料粉末包含于热塑性树脂那样的粘合剂中并进行片化,将该片与织物交替地层叠,施压,从而使骨料浸透于织物中。进一步通过将熔融金属浸渍(MI)、气相浸渍(CVI)、液相浸渍(例如聚合物熔融浸渍热分解(PIP))、固相浸渍(SPI)中的任意一种以上组合而对其进行处理,生成基质。
以下主要参照图1,说明该陶瓷基复合材料的制造工艺。基于组合了MI法的例子进行说明,但不必限定于此。
一个实施方式的陶瓷基复合材料中,可以利用由SiC构成的原料纤维。其中可以使用通过市售可获取的材料。或者,可以在原料纤维中包含由除了碳化硅(SiC)以外的其他无机物构成的纤维,或者可以用其代替SiC。
为了通过界面涂覆进行覆盖,可以对原料纤维实施涂覆。作为界面涂覆,可例示碳(C)、氮化硼(BN),但不必限定于此。就耐氧化性方面而言,BN比C更优异。作为涂覆的方法,可以利用气相法、浸渍法等任意公知方法。此外,涂覆可以在后述的纺织工序之前实施,也可以在纺织工序之后实施。界面涂覆可以防止龟裂从基质向纤维传播,增大韧性。以下的说明中,称为原料纤维时,意思包含通过界面涂覆而被覆盖的原料纤维。
将原料纤维纺织而形成织物11(织物成形工序S1)。织物11可以进行二维纺织,也可以进行三维纺织。此外,该织物11可以预先成形为根据用途确定的预定形状。由原料纤维构成的多片织物11被成形。
与织物11的成形同时准备包含骨料粉末和粘合剂的组合物1。
作为骨料,可利用陶瓷,其一个例子为SiC。为了后述的MI法,骨料粉末可以进一步含有碳(C)粉末。骨料粉末中C与SiC的比是任意的,此外,骨料粉末也可以仅为C或仅为SiC。关于骨料粉末的粒径没有特别限定,相比而言粒径小的话更容易浸渍于织物中微细的孔隙,另一方面,相比而言粒径大的话容易防止粉末的凝聚。可以基于这样的见解来选择粒径。
作为粘合剂,可以利用具有在高温时有增塑性、通过达到进一步的高温则分解消失的性质的粘合剂,作为这样的原材料,可例示出热塑性树脂。热塑性树脂典型地在200℃以上熔融、分解、蒸发,从而消失。作为热塑性树脂,可例示出苯乙烯系、丙烯酸系、纤维素系、聚乙烯系、乙烯系、尼龙系、氟化碳系树脂。
为了调整粘度、流动性的目的、以及调整形状稳定性的目的等各种目的,粘合剂可以含有添加物。作为添加物,可例示例如聚甲醛、聚丙烯、脂肪酸酯、脂肪酸酰胺、邻苯二甲酸酯、石蜡等蜡。该添加物可以仅添加一种,也可以添加选自其中的两种以上。
或者,可以利用含有这些添加物而适当进行了成分调整的市售的粉末注射成形用粘合剂。这样的粉末注射成形用粘合剂通常可以以MRM-1(IHI Turbo的商品名)的名称获取。
粘合剂相对于骨料粉末的混合比可以适当调整。关于粘合剂的混合比,相比而言大的话,对保持组合物1的形状有利,相比而言小的话,有利于将更多的骨料粉末浸透于织物11中。这里,关于粘合剂的混合比,例如相对于骨料粉末可以设为20至80体积%,更优选可以设为30至60体积%。
与图1组合而参照图2A,为了赋予适当的粘度,将含有骨料粉末和粘合剂的组合物1加热至100至150℃,并进行混炼(混炼工序S3)。为了混炼,可以利用例如具备一对螺旋轴3的双轴式混炼机,但不必须限定于此。优选地,在预先启动的混炼机中,首先投入粘合剂,确认成为适当的粘度后,缓慢投入骨料粉末。混炼耗时例如10分钟以上,尽可能将不悬浮于粘合剂中的块状粉末除去。
取出经混炼的组合物1,在保温的同时、或者再次加热到100至150℃而在模具中加压,成形为例如短圆筒状的多个片。或者,也可以通过混炼机以棒状或板状的注射物的形式射出,并连续地导入接下来的片化工序。优选地,片或注射物预备成形为接近片的形状。
与图1组合而参照图2B,注射物或预备成形物5被类似压延机的一对旋转辊7压碎。为了不粘着于辊,优选地注射物或预备成形物5被脱模片等夹持而导入到辊中。通过向下施压,使注射物或预备成形物5拉伸,成形为宽度更宽的片9(片化工序S5)。含有骨料粉末和粘合剂的多片片9分别被成形。
与图1组合而参照图3A,由原料纤维构成的织物11与含有骨料粉末和粘合剂的片9交替层叠(层叠工序S7)。层叠的织物11和片9的数量没有特别限定,为2对以上。
与图1组合而参照图3B,在100至150℃程度的温度区间,该层叠体13被类似压延机的一对旋转辊施压(施压工序S9)。也可以替代利用辊的加压而是将层叠体13封入模具15中而加压,也可以替代施加单轴压P的方式而施加多轴压或静水压。进一步,或者也可以在气密的模具中抽真空。在该工序中,骨料粉末与粘合剂一起侵入纤维间的孔隙,成为基质的原料。
在施压工序之后、或与其同时,如图4A所示那样,将层叠体13成形为成形体21。该成形可以通过例如将层叠体13加热至100至150℃程度、封入于模具中并加压来进行。按照不对成形体21造成热冲击的方式缓慢冷却后,从模具中取出。此时粘合剂为固体,因此保持被成形的形状,此外防止骨料粉末脱落。
施压工序或成形工序之后,可以进行用于将粘合剂分解的热处理(脱脂工序)。当持续进行熔融金属的浸渍时,可以如后述那样同时进行浸渍和脱脂。当单独进行脱脂时,例如在减压的炉中、或者利用非氧化性气体吹扫的炉中,利用碳加热器那样的加热手段将层叠体13或成形体21加热从而进行脱脂。加热温度至少为粘合剂的分解温度(例如250℃)以上的适当温度(例如350℃),可将其保持数小时(例如4~8小时)。粘合剂由于加热而分解、消散,从而在层叠体13或成形体21中残留原料纤维和骨料粉末。
返回来参照图1,在施压工序或成形工序之后,进行熔融金属的浸渍(浸渍工序S11)。将例如硅(Si)或Si合金的铸块附着于层叠体13或成形体21,通过加热将Si熔融而浸透。如果没有上述脱脂工序,则能够在该加热的同时引起脱脂。
加热的温度为铸块中的Si熔融的温度以上。该温度取决于铸块的组成,例如纯Si的融点为1410℃,通过合金化能够成为进一步的低温。此外,优选熔融温度为+20℃以上。如果温度过高,则增强纤维或其涂覆(coating)劣化,因此加热的温度例如为1500℃以下。典型而言,加热的温度为1390℃。
基于MI法的浸渍与烧成同时进行(烧成工序S13)。即,Si通过熔融而浸渍于层叠体13或成形体21,与骨料粉末中的C反应而生成SiC,该SiC与骨料粉末中的SiC成为一体而构成基质。加热的时间为用于熔融和反应的充分的时间,例如为10分钟以上。如果时间过长,则增强纤维或其涂覆劣化,因此加热时间例如为1小时以下。典型而言,加热时间为20分钟。
如已述的那样,可以替代MI法而利用公知的CVI法、PIP法、SPI法。此外,也可以将其中的两种以上的方法反复实施。其中,浸渍工序和烧成工序是连续进行的独立工序。
所得到的陶瓷基复合材料通常实施精加工,得到如图4B所示那样的最终制品。为了防腐蚀、提高耐热性、或防止外来物质的附着等目的,可以在精加工后进一步实施涂覆。
如已述的那样,通过以往技术、例如SPI法可以将骨料粉末浸渍到孔隙中,但由于缺乏用于浸透的驱动力,其效率不一定良好。根据本实施方式,粘合剂在施压工序中受到压力,在该压力下,以粘合剂为介质的骨料粉末和以该压力为驱动力的骨料粉末浸渍于纤维间的孔隙中。根据本实施方式,可以利用压力作为驱动力,因此骨料粉末高效地浸渍于纤维间的孔隙。不仅能够提高孔隙的堵塞率,还能够缩短工序所需要的时间。
此外,本实施方式不利用溶剂,因此不需要为了其干燥而花费的时间。粘合剂通过冷却而迅速固化,此外,通过加热而容易被除去。若利用MI法,则能够在其加热工序同时进行粘合剂的除去。与需要干燥时间的以往技术相比,在这一点上,工序所需时间缩短。
本实施方式在加工的容易性、成形的容易性和强度方面而言有利。
由于原料纤维几乎不发生伸缩,因此如果没有粘合剂,则使织物变形都不容易。织物存在着不发生随着铸模的变形而扭曲出褶皱、或者若强行进行变形则纤维局部松开的倾向。此外,如果没有用于保持形状的某些手段,则即便变形也容易回弹,无法保存形状。然而,根据本实施方式,原料纤维以被具有粘性的粘合剂限制的状态将变形增强,因此容易发生随着铸模的变形。因此,织物11不会扭曲出褶皱,也不会松开。固化了的粘合剂起到保持形状的作用。此外,如已述的那样,在成形过程中或成形后,骨料粉末也没有脱落。
陶瓷基复合材料通常在增强纤维的走向上能发挥极高的强度,然而在与此不同的方向或增强纤维不连续的方向上,仅由基质承担应力,因此强度显著差。例如当制造整体材料、并将其切削而制成最终制品形状时,有时增强纤维在多个部位不连续。根据图4B所示的汽轮机的定子叶片(stator vane)的例子,将其从整体切削的话,即使例如在叶片部25增强纤维连续,在以大致直角从此处突出的外部带27、内部带29处,增强纤维也难以连续。
根据本实施方式,如图4A所示,成形体21通过将织物弯曲而成形为接近最终制品形状的形状,纤维贯穿其整体而连续。如图4B所示,就最终制品23而言,将其成形体21烧成后仅实施极少的精加工,因此纤维的连续性不受到损害。即,该最终制品23中,增强纤维连续地从叶片部25向外部带27、以及从叶片部25向内部带29移动。可知在任意部位都能确保强度。
进一步,成形后的形状为接近制品形状的近净形状,因此精加工的负担本身也被减轻。
说明了几个实施方式,基于上述公开内容,具有本技术领域的通常技术的人能够对实施方式进行修正和变形。
产业可利用性
提供一种能够有效堵塞孔隙的陶瓷基复合材料的制造方法。
Claims (6)
1.一种陶瓷基复合材料的制造方法,包括:
将含有陶瓷的骨料粉末、与含有选自由热塑性树脂和蜡所组成的组中的一种以上的粘合剂混炼,以得到由所述骨料粉末和所述粘合剂构成的组合物,
对所述组合物施压以制成片,
将由含陶瓷的增强纤维构成的织物与所述片交替地层叠,
施压所述织物与所述片的层叠体,
生成使所述增强纤维相互结合的基质。
2.根据权利要求1所述的制造方法,其中,所述陶瓷含有SiC。
3.根据权利要求1或2所述的制造方法,其中,生成所述基质的阶段包含选自由熔融金属浸渍、气相浸渍、液相浸渍和固相浸渍所组成的组中的一种以上。
4.根据权利要求1或2所述的制造方法,其中,所述骨料粉末进一步含有碳粉末,生成所述基质的阶段包括在所述层叠体上附着由Si或Si合金形成的铸块,加热至所述铸块熔融的温度。
5.根据权利要求1或2所述的制造方法,进一步包括:
在所述施压阶段的同时、或之后,对所述层叠体进行近净成形。
6.根据权利要求1或2所述的制造方法,进一步包括:
将所述增强纤维用碳或氮化硼被覆。
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CN107734948A (zh) * | 2017-09-05 | 2018-02-23 | 西北工业大学 | 基于频率选择表面和三明治夹层结构设计的宽频带吸波材料及制备方法 |
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CN115403396A (zh) * | 2021-05-28 | 2022-11-29 | 三菱重工航空发动机株式会社 | 陶瓷基复合材料的成形方法以及陶瓷基复合材料 |
Also Published As
Publication number | Publication date |
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US20170217842A1 (en) | 2017-08-03 |
EP3199503A4 (en) | 2018-06-13 |
WO2016132821A1 (ja) | 2016-08-25 |
EP3199503A1 (en) | 2017-08-02 |
JP2016150873A (ja) | 2016-08-22 |
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