CN116375487A - 一种低孔隙率SiC纤维单向预浸带的制备方法 - Google Patents
一种低孔隙率SiC纤维单向预浸带的制备方法 Download PDFInfo
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Abstract
本发明公开了一种低孔隙率SiC纤维单向预浸带的制备方法，目的是解决如何降低单向预浸带的孔隙率的技术问题，技术方案为：在连续SiC纤维表面制备复合涂层，然后退绕到料盘上获得退绕丝，将退绕丝连同料盘密封后，置于高压釜中，导入陶瓷浆料，施加压力并保压，获得浸浆的纤维，然后缠绕到卷绕辊上，干燥后获得浆料分布均匀、低孔隙率的SiC纤维单向预浸带，层叠成型，先后经过热压罐固化、高温碳化和真空熔融渗硅后，获得MI‑SiC/SiC陶瓷基复合材料。本发明通过在带表面涂层的SiC束丝浸渍浆料阶段先抽真空再加压的工艺，除去纤维中的空气以及浆料中的气泡，使浆料充分渗入纤维束内，可以显著提高SiC纤维单向预浸带的致密度和浆料分布均匀性。
Description
技术领域
本发明属于陶瓷基复合材料制备技术领域，尤其涉及一种低孔隙率SiC纤维单向预浸带的制备方法。
背景技术
连续纤维增强陶瓷基复合材料具有耐高温、高比强度、高比模量的突出优点，且具有类似金属的断裂特征，可靠性高，因此成为新型航空航天器件热结构件及核工业抗辐射构件的急需材料(沙建军，代吉祥，张兆甫，纤维增韧高温陶瓷基复合材料(Cf,SiC/SiC)应 用研究进展，航空制造技术，2017)。
连续碳化硅纤维增强碳化硅陶瓷基复合材料(SiC/SiC)是目前耐高温性能最优异的结构材料之一。该材料的制备方法主要有以下几种(刘虎，杨金华，焦健，航空发动机用连 续SiC/SiC复合材料制备工艺及应用前景，航空制造技术，2017)：化学气相渗透法(ChemicalVaporInfiltration，CVI)、熔融浸渗法(MeltInfiltration，MI)、纳米渗透瞬态共晶法(Nano-InfiltrationandTransientEutectic，NITE)、溶胶-凝胶法(Sol-Gel)、先驱体浸渍裂解法(PrecursorImpregnationandPyrolysis，PIP)、CVI+PIP及NITE+PIP等组合制备工艺。
在这些技术中，MI工艺制备的SiC/SiC复合材料(MI-SiC/SiC)具有孔隙率低、导热率高、层间剪切强度高等性能优势，且该工艺还有制备周期短、成本低的突出优点，因此已在国外应用于制造航空发动机和工业燃气轮机热端构件。
美国通用电气(GE)公司开发了单向预浸带-熔渗(Prepreg-MI)工艺，并发展了以
为牌号的MI-SiC/SiC复合材料产品，已经成功应用于航空发动机及工业燃气轮机的涡轮外环、燃烧室等热结构件(董绍明，胡建宝，张翔宇，SiC/SiC复合材料MI工艺 制备技术，航空制造技术，2014，6)。单向预浸带-MI工艺主要包括以下步骤：(1)首先采用化学气相沉积(CVD)技术在SiC纤维表面制备界面层；(2)将SiC粉体、碳粉体与树脂粘结剂、表面活性剂与溶剂混合，制备成陶瓷浆料，使浆料浸入带涂层的SiC纤维束，湿法卷绕形成SiC纤维单向预浸带；(3)单向预浸带层叠后形成复合材料预制体，然后经过固化实现定型；(4)热解将树脂碳化，其它有机组分以气态排出，形成带有大量微孔的预制体，为后续渗硅提供通道；(5)最后将硅粉或硅块升温至熔融状态(＞1410℃)，液态硅在毛细管力的作用下渗入多孔的纤维预制体，硅和碳反应生成碳化硅，制备出致密的MI-SiC/SiC复合材料。
在上述MI过程中，熔融硅在毛细管力作用下进入基体内部，液硅与预制体内部的碳发生反应，生成SiC。反应式如下：
Si(l)+C(s)＝SiC(s)
冷却后，MI-SiC/SiC的基体由预制体中加入的SiC粉体、熔融硅与碳反应生成的SiC以及少量的残余硅(～5％)组成，此外基体中还含有2％～5％的孔隙。
MI-SiC/SiC主要用于高温氧化服役环境中，要求孔隙率尽量低。孔隙除了会显著降低复合材料的强度、弹性模量、导热率外，还会严重损害复合材料的高温抗氧化性，甚至为氧化性气氛到达复合材料内部提供扩散通道，导致复合材料内氧化，产生脆性断裂，严重降低服役可靠性。
MI-SiC/SiC复合材料的孔隙主要来源之一是在制备SiC纤维单向预浸带的时候，陶瓷浆料无法完全浸入到纤维束中(一般商品化的连续SiC纤维规格是每束纤维含有500根单丝，每根单丝直径约为15μm)，从而形成孔隙。该孔隙在后续热压罐致密化过程中会部分愈合，但是很难完全消除。在熔融渗硅时，在含有较大孔的部位毛细管力较低，不容易填充，导致最终MI-SiC/SiC复合材料中残存孔隙。
当采用美国GE公司的技术路线制备MI-SiC/SiC时，是将带有涂层的SiC纤维束丝连续通过常压下的浆料槽，浆料渗透到SiC纤维束丝中，然后单层排布在卷绕辊上形成单向预浸带。
由于陶瓷浆料粘度较高、SiC纤维束丝中单丝之间的空隙小、SiC纤维束丝通过浆料槽的时间短(1～5秒)、浆料中含有气泡等因素，浆料经常无法完全浸透到SiC纤维束丝内，干燥后的单向预浸带含有一定量的孔隙。因此如何降低单向预浸带的孔隙率是制备高质量MI-SiC/SiC复合材料的关键技术之一。
发明内容
本发明的目的在于提供一种低孔隙率SiC纤维单向预浸带的制备方法，以解决上述技术问题。
本发明为解决上述技术问题，采用以下技术方案来实现：
一种低孔隙率SiC纤维单向预浸带的制备方法，包括如下步骤：
1)在连续SiC纤维表面制备复合涂层，获得带涂层的连续纤维A；
2)将A退绕到料盘上，获得退绕丝B；
3)将B连同料盘一同置于高压釜中，密封后，先对高压釜抽真空，然后将陶瓷浆料导入釜中，液面完全覆盖纤维，最后对釜内施加压力并保压，获得浸浆的纤维C；
4)将C从高压釜中取出，将充分浸渍陶瓷浆料的连续纤维在湿态下单层缠绕到卷绕辊上，干燥后，获得浆料分布均匀、低孔隙率的SiC纤维单向预浸带D；
5)将D层叠成型，先后经过热压罐固化、惰性气氛下高温碳化和真空熔融渗硅后，获得MI-SiC/SiC陶瓷基复合材料E。
优选的，所述步骤1)中复合涂层从纤维表层向外依次为BN涂层、Si3N4涂层和C涂层，采用化学气相沉积方法制备而成。
优选的，所述BN涂层的厚度为200nm-600nm，所述Si3N4涂层的厚度为100nm-500nm，所述C涂层的厚度为5nm-50nm。
优选的，所述步骤3)中陶瓷浆料中包括碳化硅粉体、碳粉体、树脂粘合剂、分散剂及溶剂，所述高压釜中抽真空的压力为-0.1MPa，加压压力范围为3MPa-6Mpa，保压10min。
优选的，所述陶瓷浆料的固含量为20％-50％，所述碳化硅粉体的粒度为0.5μm-5μm，所述碳粉体的粒度为0.1μm-5μm，所述树脂粘合剂为环氧树脂、酚醛树脂或者糠醛树脂中的任意一种。
优选的，所述步骤4)中SiC纤维单向预浸带D的单片厚度为0.2mm-0.6mm。
优选的，所述步骤5)中热压罐的固化压力为0.5MPa-2MPa；温度为80℃-150℃，保温时间为0.5h-10h；高温碳化在任一惰性气氛中进行，温度为900℃-1300℃，保温时间为0.5h-5h；熔融渗硅温度为1410℃-1450℃，渗硅时间为1min-60min。
本发明的有益效果是：
1、本发明通过在带表面涂层的SiC束丝浸渍浆料阶段先抽真空再加压的工艺，除去纤维中的空气以及浆料中的气泡，使浆料充分渗入纤维束内，可以显著提高SiC纤维单向预浸带的致密度和浆料分布均匀性；
2、本发明的单向预浸带可显著提高MI-SiC/SiC复合材料的性能一致性，从而提高MI-SiC/SiC构件的服役可靠性；
3、本发明工艺简单、成本低，适于批量生产，具有工程化应用的价值。
附图说明
图1为带涂层纤维退绕至料盘示意图；
其中：1-纤维筒，2-退绕***的布丝头，3-料盘。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例和附图，进一步阐述本发明，但下述实施例仅仅为本发明的优选实施例，并非全部。基于实施方式中的实施例，本领域技术人员在没有做出创造性劳动的前提下所获得其它实施例，都属于本发明的保护范围。
下面结合附图描述本发明的具体实施例。
实施例1
一种低孔隙率SiC纤维单向预浸带的制备方法，包括如下步骤：
1)在连续SiC纤维表面利用CVD法制备厚度为400nm的BN界面层，BN层在复合材料中承担传递载荷、裂纹偏转、纤维脱粘等作用，在BN界面层表面制备厚度为400nm的Si3N4涂层，用于抵抗熔融渗硅时液硅对BN涂层及SiC纤维的腐蚀损伤；最后在Si3N4涂层表面制备厚度为30nm的热解碳界层，以促进液态硅渗入到预制体中，获得带复合涂层的连续SiC纤维A；
2)将带涂层的连续SiC纤维A退绕到不锈钢料盘中，获得退绕丝B；退绕时应避免纤维束的密堆积，从而影响后续浆料的浸透。
3)将退绕丝B连同料盘一同置于高压釜中，密封后，先对高压釜抽真空至-0.1MPa，然后将含有碳化硅粉体、碳粉体、树脂粘合剂、分散剂及溶剂的陶瓷浆料导入釜中，液面完全覆盖纤维，最后对釜内施加压力至3MPa并保压10min，获得浸浆的纤维C；
陶瓷浆料中含有25wt.％的SiC粉体，粒径(D50)为0.8μm；10wt.％的C粉体，粒径(D50)为0.1μm；12wt.％的酚醛树脂及固化剂；3wt.％的分散剂聚乙烯亚胺(PEI)；溶剂为无水乙醇。
4)将C从高压釜中取出，将充分浸渍陶瓷浆料的连续纤维在湿态下单层缠绕到直径为400mm，长度为600mm的卷绕辊上，干燥后，获得长度为1256mm，宽度为500mm，厚度为0.3mm，浆料分布均匀、低孔隙率的SiC纤维单向预浸带D；
5)将D剪裁成200mm×200mm的片材，将八片D层叠形成预制体，其中两层相邻D之间纤维的排列方向互相垂直；将预制体利用真空袋密封，内部持续抽真空，置于热压罐中固化，固化压力为1.2MPa，固化温度为130℃，固化时间为2h，获得固化后的预制体，此时预制体的尺寸为200mm×200mm×2.8mm，固化后的预制体在N2气氛中1100℃热处理1h，获得碳化后的预制体，在此过程中，碳基树脂粘合剂在高温下发生碳化，排除气体副产物，在基体中引入大量孔道，为后续的熔融渗硅提供了通路；最后，在10Pa真空下1440℃熔融渗硅，保温30min，而后随炉冷却至室温，当硅在高温下熔融后，在毛细管力的作用下渗透入预制体，并与预制体层中的碳反应生成SiC，余下的少量空隙被液硅填充，获得MI-SiC/SiC复合材料。
所述BN涂层的厚度还可以为200nm-600nm之间的任意数值，所述Si3N4涂层的厚度还可以为100nm-500nm之间的任意数值，所述C涂层的厚度还可以为5nm-50nm之间的任意数值。
步骤3)中的加压压力范围还可以为2MPa-10Mpa之间的任意数值。
所述陶瓷浆料的固含量还可以为20％-50％之间的任意数值，所述碳化硅粉体的粒度还可以为0.5μm-5μm之间的任意数值，所述碳粉体的粒度还可以为0.1μm-5μm之间的任意数值，所述树脂粘合剂为环氧树脂、酚醛树脂或者糠醛树脂中的任意一种。
所述步骤4)中SiC纤维单向预浸带D的单片厚度还可以为0.2mm-0.6mm之间的任意数值。
所述步骤5)中热压罐的固化压力为0.5MPa-2MPa之间的任意数值，温度为80℃-150℃之间的任意数值，保温时间为0.5h-10h之间的任意数值，高温碳化在任意一种惰性气氛中进行，温度为900℃-1300℃之间的任意数值，保温时间为0.5h-5h之间的任意数值，熔融渗硅的温度为1410℃-1450℃之间的任意数值，渗硅时间为1min-60min之间的任意数值。
本实施例所得的MI-SiC/SiC复合材料的孔隙率为1.8％，SiC纤维的体积分数为24％，复合材料的拉伸强度为351MPa，断裂应变为0.62％，具有优异的力学性能。
实施例2
1)同实施例1的步骤1)；
2)同实施例1的步骤2)；
3)将B连同料盘置于高压釜中，密封后，先对釜抽真空至-0.1MPa，而后将含有SiC粉体和C粉体的陶瓷浆料导入釜中，液面完全覆盖纤维；利用空压机对釜内施加压力至6MPa，并保压10min，获得浸浆的纤维C，浆料配方同实施例1的步骤3)；
4)同实施例1的步骤4)；
5)同实施例1的步骤5)。
本实施例所得的MI-SiC/SiC复合材料的孔隙率为0.9％，SiC纤维的体积分数为24％，复合材料的拉伸强度为360MPa，断裂应变为0.71％，具有优异的力学性能。
与实施例1结果相比，该复合材料孔隙率更低，说明增加浸渍压力有利于纤维预制体中浆料的均匀浸润，最终提高复合材料力学性能。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的仅为本发明的优选例，并不用来限制本发明，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (7)
1.一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，包括如下步骤：
1)在连续SiC纤维表面制备复合涂层，获得带涂层的连续纤维A；
2)将A退绕到料盘上，获得退绕丝B；
3)将B连同料盘一同置于高压釜中，密封后，先对高压釜抽真空，然后将陶瓷浆料导入釜中，液面完全覆盖纤维，最后对釜内施加压力并保压，获得浸浆的纤维C；
4)将C从高压釜中取出，将充分浸渍陶瓷浆料的连续纤维在湿态下单层缠绕到卷绕辊上，干燥后，获得浆料分布均匀、低孔隙率的SiC纤维单向预浸带D；
5)将D层叠成型，先后经过热压罐固化、惰性气氛下高温碳化和真空熔融渗硅后，获得MI-SiC/SiC陶瓷基复合材料E。
2.根据权利要求1所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述步骤1)中复合涂层从纤维表层向外依次为BN涂层、Si3N4涂层和C涂层，采用化学气相沉积方法制备而成。
3.根据权利要求2所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述BN涂层的厚度为200nm-600nm，所述Si3N4涂层的厚度为100nm-500nm，所述C涂层的厚度为5nm-50nm。
4.根据权利要求1所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述步骤3)中陶瓷浆料中包括碳化硅粉体、碳粉体、树脂粘合剂、分散剂及溶剂，所述高压釜中抽真空的压力为-0.1MPa，加压压力范围为3MPa-6MPa，保压10min。
5.根据权利要求4所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述陶瓷浆料的固含量为20％-50％，所述碳化硅粉体的粒度为0.5μm-5μm，所述碳粉体的粒度为0.1μm-5μm，所述树脂粘合剂为环氧树脂、酚醛树脂或者糠醛树脂中的任意一种。
6.根据权利要求1所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述步骤4)中SiC纤维单向预浸带D的单片厚度为0.2mm-0.6mm。
7.根据权利要求1所述的一种低孔隙率SiC纤维单向预浸带的制备方法，其特征在于，所述步骤5)中热压罐的固化压力为0.5MPa-2MPa；温度为80℃-150℃，保温时间为0.5h-10h；高温碳化在任一惰性气氛中进行，温度为900℃-1300℃，保温时间为0.5h-5h；熔融渗硅温度为1410℃-1450℃，渗硅时间为1min-60min。
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