CN113307643B - 一种基于单向带SiCf/SiC复合材料制备方法 - Google Patents

一种基于单向带SiCf/SiC复合材料制备方法 Download PDF

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CN113307643B
CN113307643B CN202110612761.2A CN202110612761A CN113307643B CN 113307643 B CN113307643 B CN 113307643B CN 202110612761 A CN202110612761 A CN 202110612761A CN 113307643 B CN113307643 B CN 113307643B
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刘时剑
邱海鹏
刘善华
陈明伟
谢巍杰
张冰玉
关宏
王启明
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
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Abstract

本发明涉及一种基于单向带SiCf/SiC复合材料制备方法。首先将单向SiC纤维带制备成带界面层的预浸料，通过热压定型方法，将若干层单向SiC纤维预浸料制备成SiCf/SiC‑C多孔成型体，然后通过高温熔渗，制备出致密SiCf/SiC复合材料。本发明通过采用热熔纱‑单向SiC纤维带进行预浸料‑熔渗工艺研究，避免了SiC纤维在预制体编织过程中卷曲所带来的纤维损伤；通过制备专用预浸浆料组分，解决了热熔纱高温分解导致纤维松散难以成型的问题；本发明方法制备的复合材料在相同厚度下，相比传统平纹布铺层具有更低的纤维含量，降低了复合材料制备的成本，具有工程化的应用前景。

Description

一种基于单向带SiCf/SiC复合材料制备方法
技术领域
本发明涉及复合材料制备技术领域，特别是涉及一种基于单向带 SiCf/SiC复合材料制备方法。
背景技术
SiCf/SiC复合材料作为陶瓷基复合材料的典型代表，具有高强高模、低密及高温抗氧化等优异性能，是航空航天领域热端构件的潜在应用材料之一。相较于先驱体浸渍裂解(PIP)和化学气相沉积(CVI)，用熔渗工艺(MI)制备SiCf/SiC复合材料具有成本低，周期短，致密度高，孔隙率低等特点。预浸料-熔渗工艺是一种基于熔渗工艺开发出来的新型工艺，其流程为单丝束SiC纤维通过连续丝束界面沉积炉制备界面层，经过预浸机料槽挂上浆料，通过湿滚缠绕法制备出预浸料的单向SiC纤维带，然后叠层热压形成SiCf/SiC复合材料的多孔坯体，最后通过熔融渗硅进行致密化。由于复合材料是单向纤维带铺层而来，纤维不存在卷曲、弯折等问题，使得复合材料在纤维方向上的力学性能较优异。近几年，我国已开始开展预浸料-熔渗工艺制备陶瓷基复合材料的相关研究。专利 201810268751.X介绍了一种基于预浸料SiC纤维二维布的SiCf/SiC复合材料熔渗制备技术。该方法以SiC纤维作为增强体，首先在SiC纤维二维布表面制备界面层，进而通过PCS前驱体浸渍裂解法进行预制体定型、再通过熔融渗硅的方法实现材料的致密化，制备出SiCf/SiC复合材料。专利201910663654.5和专利201910618382.7均介绍了一种基于预浸料-熔渗的技术，该方法均是将浆料涂覆在SiC纤维二维布上，常温晾干得到纤维预浸料，然后通过铺层、热压、碳化以及熔渗制备成SiCf/SiC复合材料。
可以发现，目前主流的研究方向是利用SiC纤维二维布研究预浸料-熔渗工艺中的后续步骤，如铺层成型，熔渗等。这是由于现有的技术以及设备均处于空白状态，无法对连续SiC单丝束纤维沉积界面层以及制备成单向带。SiC纤维二维布由于经、纬两向纤维的交叉缠绕，会损耗SiC纤维的力学性能，影响最终复合材料的性能；同时经纬纤维交叉节点的位置易产生孔隙等缺陷，影响复合材料整体致密度。研究基于单向SiC纤维带的预浸料-熔渗工艺是必然趋势。
因此，发明人提供了一种基于单向带SiCf/SiC复合材料制备方法。
发明内容
(1)要解决的技术问题
本发明实施例提供了一种基于单向带SiCf/SiC复合材料制备方法，解决了现有技术制备的SiCf/SiC复合材料在预制体编织过程中因卷曲所带来的纤维损伤，导致纤维方向上力学性能较差，同时经纬纤维交叉节点的位置易产生孔隙等缺陷，影响复合材料整体致密的问题。
(2)技术方案
本发明的实施例提出了一种基于单向带SiCf/SiC复合材料制备方法，包括以下步骤S110～步骤S160：
步骤S110，制备界面相：用模具将单层的热熔纱-单向SiC纤维带夹好，放入界面层沉积炉中，制备氮化硼界面相。
步骤S120，制备预浸浆料：用SiC粉体、有机碳源以及有机溶剂按 3:5:2的比例配置预浸浆料，经球磨6h～48h后得到混合均匀的预浸浆料。
步骤S130，制备单向SiC纤维预浸料：将步骤S110中带模具的含有氮化硼界面相的单向SiC纤维带放入真空容器中浸渍，先抽真空，后灌入步骤S120制备的预浸浆料，保压4h～12h后取出，放入烘箱烘干后，脱模得到单向SiC纤维预浸料。
步骤S140，叠层热压成型：将5～20层步骤S130得到的单向SiC纤维预浸料带的两面涂刷粘接剂，并按照纤维布的方向铺叠，通过热压工艺固化成型得到多孔成型体。
步骤S150，高温裂解：将步骤S140得到的多孔成型体放置于高温裂解炉中进行裂解，自然冷却后得到SiCf/SiC-C多孔体。
步骤S160，高温熔渗：将步骤S150得到的SiCf/SiC-C多孔体放入熔渗炉中，并用Si粉包埋进行高温熔渗，自然冷却后，得到致密SiCf/SiC复合材料。
进一步地，所述步骤S110中，所述热熔纱-单向SiC纤维带的经向是 SiC纤维，纬向是热熔纱，织物组织为平纹。
进一步地，所述步骤S110中，所述氮化硼界面相的厚度为 100nm～500nm。
进一步地，所述步骤S120中，所述有机碳源为呋喃树脂、糠酮树脂、酚醛树脂中的至少一种，所述有机溶剂为乙醇或丙酮。
进一步地，所述步骤S130中，放入烘箱烘干的条件为：加热至 160℃～240℃，保温2h～24h。
进一步地，所述步骤S140中，所述粘接剂为呋喃树脂、酚醛树脂、液态聚碳硅烷中的一种。
进一步地，所述步骤S140中，通过热压工艺固化成型的条件是：以 5℃/min～10℃/min的升温速率从室温加热到160℃～240℃，压力为 2MPa～4MPa，保温0.5小时～2小时。
进一步地，所述步骤S150中，高温裂解炉中进行裂解的条件为：以 100℃/h～600℃/h的升温速率从室温加热到800℃～1200℃，保温0.5h～2h，压力为真空。
进一步地，所述步骤S150中，放入熔渗炉中进行高温熔渗的条件为：以100℃/h～600℃/h的升温速率从室温加热到1410℃～1500℃，保温1 小时～4小时，压力为真空。
(3)有益效果
首先，本发明利用了热熔纱高温分解的特点，热熔纱在复合材料界面层沉积升温过程中就能完全分解，不影响后续工艺且不引入杂质，使得 SiC纤维单向地保留在复合材料中，达到单向SiC纤维带作为增强体的效果。
其次，由于热熔纱-单向SiC纤维带在制备界面层后，热熔纱分解，单向SiC纤维之间不存在结合力，会分散，进而影响后续成型工艺。本发明通过设计专用的浆料组分，使得分散的SiC纤维在预浸料后可以通过浆料基体进行固定，脱模后纤维不松散，确保后续热压成型工艺的可行性。
最后，相比于传统的SiC纤维二维布，本发明基于热熔纱-单向SiC纤维带制备的复合材料具有更低的纤维体积分数，降低了SiCf/SiC复合材料的制备成本，采用本发明方法制备的SiCf/SiC复合材料力学性能较好，整体致密性更好。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对本发明实施例中所需要使用的附图作简单地介绍，显而易见地，下面所描述的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实施例的一种基于单向带SiCf/SiC复合材料制备方法的工艺流程图。
具体实施方式
下面结合附图和实施例对本发明的实施方式作进一步详细描述。以下实施例的详细描述和附图用于示例性地说明本发明的原理，但不能用来限制本发明的范围，即本发明不限于所描述的实施例，在不脱离本发明的精神的前提下覆盖了设备和操作方式的任何修改、替换和改进。
需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的特征可以相互组合。下面将参照附图并结合实施例来详细说明本申请。
实施例1
请参照图1所示，本发明提供了一种基于单向带SiCf/SiC复合材料制备方法，该制备方法包括以下步骤S110～步骤S160：
步骤S110，制备界面相：用模具将单层的热熔纱-单向SiC纤维带夹好，放入界面层沉积炉中，制备氮化硼(BN)界面相，所述氮化硼界面相的厚度为200nm。
在该步骤中，热熔纱-单向SiC纤维带的经向采用了国产SiC纤维，纬向是热熔纱，织物组织为平纹。
步骤S120，制备预浸浆料：用30份的SiC粉体、50份的有机碳源以及20份的有机溶剂配置预浸浆料，经球磨24h后得到混合均匀的预浸浆料。本实施例中，有机碳源采用呋喃树脂，有机溶剂采用丙酮。
步骤S130，制备单向SiC纤维预浸料：将步骤S110中带模具的含有氮化硼界面相的单向SiC纤维带放入真空容器中浸渍，先抽真空，后灌入步骤S120制备的预浸浆料，保压10h后取出，放入烘箱，加热至200℃，保温4h，烘干后，脱模得到单向SiC纤维预浸料。
步骤S140，叠层热压成型：将10层步骤S130得到的单向SiC纤维预浸料带的两面涂刷粘接剂，并按照纤维布的方向[0°-90°-0°-90°](即按照第一层纤维带沿长度为横向铺叠，下一层纤维带沿长度为纵向铺叠，相邻两层纤维带是交叉方向铺叠)的顺序铺叠，以10℃/min的升温速率从室温加热到200℃，压力为3MPa，保温2小时，通过热压工艺固化成型得到多孔成型体。本实施例中的粘接剂采用呋喃树脂。
步骤S150，高温裂解：将步骤S140得到的多孔成型体放置于高温裂解炉中进行真空裂解，以300℃/h的升温速率从室温加热到1200℃，保温 1h，自然冷却后得到SiCf/SiC-C多孔体。
步骤S160，高温熔渗：将步骤S150得到的SiCf/SiC-C多孔体放入熔渗炉中，并用Si粉包埋，以300℃/h的升温速率从室温加热到1450℃，保温2小时，压力为真空，进行高温熔渗，自然冷却后，得到致密SiCf/SiC 复合材料。
经测试，所制备的SiCf/SiC复合材料密度密度2.65g/cm3，孔隙率 3.9％，0°方向的拉伸强度283MPa。
实施例2
步骤S110，制备界面相：用模具将单层的热熔纱-单向SiC纤维带夹好，放入界面层沉积炉中，制备氮化硼(BN)界面相，所述氮化硼界面相的厚度为200nm。
在该步骤中，热熔纱-单向SiC纤维带的经向采用了国产SiC纤维，纬向是热熔纱，织物组织为平纹。
步骤S120，制备预浸浆料：用30份的SiC粉体、50份的有机碳源以及20份的有机溶剂配置预浸浆料，经球磨24h后得到混合均匀的预浸浆料。本实施例中，有机碳源采用呋喃树脂，有机溶剂采用丙酮。
步骤S130，制备单向SiC纤维预浸料：将步骤S110中带模具的含有氮化硼界面相的单向SiC纤维带放入真空容器中浸渍，先抽真空，后灌入步骤S120制备的预浸浆料，保压10h后取出，放入烘箱，加热至200℃，保温4h，烘干后，脱模得到单向SiC纤维预浸料。
步骤S140，叠层热压成型：将10层步骤S130得到的单向SiC纤维预浸料带的两面涂刷粘接剂，并按照纤维布的方向[0°-0°-90°-0°-0°-90°] (即，按照前两层纤维带沿长度为横向铺叠，下一层纤维带沿长度为纵向铺叠，然后再两层纤维带沿长度为横向铺叠，相邻两层纤维带是交叉方向铺叠)的顺序铺叠，以10℃/min的升温速率从室温加热到200℃，压力为 3MPa，保温2小时，通过热压工艺固化成型得到多孔成型体。本实施例中的粘接剂采用呋喃树脂。
步骤S150，高温裂解：将步骤S140得到的多孔成型体放置于高温裂解炉中进行真空裂解，以300℃/h的升温速率从室温加热到1200℃，保温 1h，自然冷却后得到SiCf/SiC-C多孔体。
步骤S160，高温熔渗：将步骤S150得到的SiCf/SiC-C多孔体放入熔渗炉中，并用Si粉包埋，以300℃/h的升温速率从室温加热到1450℃，保温2小时，压力为真空，进行高温熔渗，自然冷却后，得到致密的 SiCf/SiC复合材料。
经测试，所制备的SiCf/SiC复合材料密度密度2.68g/cm3，孔隙率 3.2％，0°方向的拉伸强度为311MPa。
对成型后的复合材料叶片10进行外观质量、内部质量检测，均满足设计要求。
以上所述仅为本申请的实施例而已，并不限制于本申请。在不脱离本发明的范围的情况下对于本领域技术人员来说，本申请可以有各种更改和变化。凡在本申请的精神和原理之内所作的任何修改、等同替换、改进等，均应包含在本申请的权利要求范围内。

Claims (1)

1.一种基于单向带SiCf/SiC复合材料制备方法，其特征在于，包括：
步骤S110，制备界面相：用模具将单层的热熔纱-单向SiC纤维带夹好，放入界面层沉积炉中，制备氮化硼界面相；所述热熔纱-单向SiC纤维带的经向是SiC纤维，纬向是热熔纱，织物组织为平纹；所述氮化硼界面相的厚度为100nm～500nm；
步骤S120，制备预浸浆料：用SiC粉体、有机碳源以及有机溶剂按3:5:2的比例配置预浸浆料，经球磨后得到混合均匀的预浸浆料；所述有机碳源为呋喃树脂、糠酮树脂、酚醛树脂中的至少一种，所述有机溶剂为乙醇或丙酮；
步骤S130，制备单向SiC纤维预浸料：将步骤S110中带模具的含有氮化硼界面相的单向SiC纤维带放入真空容器中浸渍，先抽真空，后灌入步骤S120制备的预浸浆料，保压4h～12h后取出，放入烘箱烘干后，脱模得到单向SiC纤维预浸料；放入烘箱烘干的条件为：加热至160℃～240℃，保温2h～24h；
步骤S140，叠层热压成型：将5～20层步骤S130得到的单向SiC纤维预浸料带的两面涂刷粘接剂，并按照纤维布的方向铺叠，通过热压工艺固化成型得到多孔成型体；所述粘接剂为呋喃树脂、酚醛树脂、液态聚碳硅烷中的一种；通过热压工艺固化成型的条件是：以5℃/min～10℃/min的升温速率从室温加热到160℃～240℃，压力为2MPa～4MPa，保温0.5小时～2小时；
步骤S150，高温裂解：将步骤S140得到的多孔成型体放置于高温裂解炉中进行裂解，自然冷却后得到SiCf/SiC-C多孔体；高温裂解炉中进行裂解的条件为：以100℃/h～600℃/h的升温速率从室温加热到800℃～1200℃，保温0.5h～2h，压力为真空；
步骤S160，高温熔渗：将步骤S150得到的SiCf/SiC-C多孔体放入熔渗炉中，并用Si粉包埋进行高温熔渗，自然冷却后，得到致密SiCf/SiC复合材料；放入熔渗炉中进行高温熔渗的条件为：以100℃/h～600℃/h的升温速率从室温加热到1410℃～1500℃，保温1小时～4小时，压力为真空。
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