CN105967712A - 碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法 - Google Patents

碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法 Download PDF

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CN105967712A
CN105967712A CN201610277281.4A CN201610277281A CN105967712A CN 105967712 A CN105967712 A CN 105967712A CN 201610277281 A CN201610277281 A CN 201610277281A CN 105967712 A CN105967712 A CN 105967712A
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李爱军
吴彪
彭雨晴
白瑞成
贾林涛
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Abstract

本发明公开了一种碳纤维增强碳化硅（Csf/C‑SiC）复合材料的制备方法，其步骤：(1)将3‑30mm短切碳纤维放在二甲亚砜溶液中，浸泡2h，除胶；(2)将短切碳纤维进行强力分散，得到分散后的短切碳纤维；(3)称取的碳化硅(SiC)粉末置于有机溶剂溶液中，搅拌下向该溶液中加入聚碳硅烷、硅粉、铝粉、硼粉，混合后得到悬浮液；(4)将悬浮液加热至80℃～120℃，蒸发，得到块状混合物，将混合物研磨，过200目以下的筛,得到混合粉末；(5)将分散后的短切碳纤维和上述混合粉末捣碎、混合，得泥浆；(6).将泥浆置于模具定型，再进行热压烧结，制得碳纤维增强碳化硅（Csf/C‑SiC）复合材料。该方法能提高材料在高温服役环境下高温性能材料的致密化度。

Description

碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法
技术领域
本发明涉及到一种热压烧结工艺制备碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，尤其涉及一种残余硅少、高温摩擦性能良好的碳纤维增强碳化硅（Csf/C-SiC）复合材料。
背景技术
热压烧结(Hot pressed sintering)是目前制造SiC及其复合材料工程器件应用最广泛的快速烧结方法。但是，碳化硅陶瓷具有很高的缺陷敏感性，韧性不足被认为陶瓷类材料的最致命缺陷，因此其应用范围受到极大的限制。
目前，引入纤维作为增强体是提高碳化硅陶瓷材料韧性和强度的有效方法。但是，由于连续纤维增强的复合材料制备工艺复杂，技术难度大，且成本较高。因此，出现了以短纤维作为增韧体的复合材料，以硅、铝、硼做烧结剂能有效降低烧结温度，提高材料致密度。但是，短切纤维与粉体的均匀混合在技术上存在较多困难，以硅为烧结助剂的热压烧结方法制备的Csf/C-SiC复合材料中残余硅较高，该材料致密度下降，尤其是在高温环境下的力学性能会显著下降。
发明内容
针对现有技术存在的不足，本发明的目的是提出一种碳纤维增强碳化硅（Csf/C-SiC）复合材料的材料制备方法，该方法制备的材料在高温服役环境下能够明显地提高材料高温性能，在烧结过程中聚碳硅烷裂解产生的微晶可有效填充基体微孔，提高材料的致密度。
为达到上述目的，本发明采用如下技术方案。
一种以聚碳硅烷为前驱体制备碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其特征在于该方法的具体步骤为：
(1). 将3-30mm短切碳纤维放在二甲亚砜溶液中，浸泡2h，进行除胶；
(2). 将除胶后的短切碳纤维进行强力分散，得到分散后的短切碳纤维；
(3)称取一定量的碳化硅(SiC)粉末置于有机溶剂溶液中，搅拌状态下依次向该溶液中加入聚碳硅烷、硅粉、铝粉、硼粉，混合均匀后得到悬浮液；
(4). 将上述步骤(3)中得到的悬浮液加热至80℃～120℃，进行蒸发，直到溶剂完全挥发，得到块状混合物，将块状混合物研磨，过200目以下的筛,得到混合粉末；
(5). 将上述步骤(1)中得到的分散后的短切碳纤维和上述步骤(4)中得到的混合粉末捣碎、混合，得混合均匀的泥浆；
(6). 将上述步骤(5)中得到混合均匀的泥浆置于石墨模具中进行冷压定型，再置于真空热压炉中，在氩气气氛中，加热至300℃，再以1～５℃/min的升温速度，压力为12.4MPa．加热至300℃～1000℃，并且在压力为26.5MPa、温度为1000℃～1900℃下恒温2～4h进行热压烧结，烧结后，自然降温至室温，制得碳纤维增强碳化硅（Csf/C-SiC）复合材料。
步骤(1)中所述的碳纤维为聚丙烯氰基碳纤维、沥青基碳纤维中的一种或几种。
步骤(2)中所述的碳纤维的体积分数为40vol%-60vol%，强力分散后短纤维长度为1mm-5mm。
步骤(3)中所述的SiC质量占碳纤维增强碳化硅复合材料质量的40-50份，聚碳硅烷占碳纤维增强碳化硅复合材料质量的0-20份，烧结助剂占碳纤维增强碳化硅复合材料质量的5-15份（其中硅粉占碳纤维增强碳化硅复合材料质量的65%-75%，铝粉占碳纤维增强碳化硅复合材料质量的20%-30%，硼粉占碳纤维增强碳化硅复合材料质量的1%-5%）。
步骤(3)中所述的有机溶剂为正己烷、二甲苯中的一种。
本发明的有益效果是，
本发明制备的碳纤维增强碳化硅（Csf/C-SiC）复合材料改善了材料在高温服役环境下的力学性能；该方法在烧结Csf/C-SiC复合材料过程中，聚碳硅烷裂解生成的游离碳与残余硅反应，能避免残余硅对纤维的侵蚀，提高材料高温性能；该方法在聚碳硅烷前驱体烧结过程中具有液相烧结作用，聚碳硅烷裂解所产生的微晶可有效填充基体微孔，提高材料的致密化度。
附图说明
　　图1为本发明制备的碳纤维增强碳化硅（Csf/C-SiC）复合材料的SEM电镜图。
具体实施方式
　　现将本发明的具体实施例综述于后。
实施例
一种以聚碳硅烷为前驱体制备碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其具体步骤为：
(1). 将9g 的3-30mm短切聚丙烯腈基碳纤维放在二甲亚砜溶液(3vol%)中浸泡2h，进行除胶；
(2). 将除胶后的短切碳纤维进行强力分散，得到分散后的短切碳纤维；
(3). 称取16g的碳化硅SiC粉末置于乙醇溶液中，并在搅拌状态下依次向该溶液中加入1.6g～4 g的聚碳硅烷、1.6g的硅粉、0.8g的铝粉、0.096g的硼粉，混合均匀后得到乙醇悬浮液；
(4). 将上述步骤(3)中得到混合均匀的乙醇悬浮液加热至150℃蒸发，直到溶剂完全挥发，得到块状混合物，将该块状混合物研磨，至200目以下的筛,得到混合粉末；
(5). 将上述步骤(1)中得到的分散后的短切碳纤维和上述步骤(4)中得到的混合粉末捣碎、混合，得混合均匀的泥浆；
(6)将上述步骤(5)中得到混合均匀的泥浆置于石墨模具中进行冷压定型，再置于真空炉中，在氩气气氛下，加热至300℃，再以2℃/min的升温速度，压力为12.4MPa．加热至300℃～1000℃，并且在压力为26.5MPa，1000℃下恒温２小时,再以5℃/min的升温速度，加热至 1800℃下恒温２小时进行热压烧结，烧结后，自然降温至室温，制得碳纤维增强碳化硅（Csf/C-SiC）复合材料，如图1所示。

Claims (4)

1.一种碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其特征在于,该方法的具体步骤为：
(1).将3-30mm短切碳纤维放在二甲亚砜溶液中，浸泡2h，进行除胶；
将除胶后的短切碳纤维进行强力分散，得到分散后的短切碳纤维；
称取一定量的碳化硅(SiC)粉末置于有机溶剂溶液中，搅拌状态下依次向该溶液中加入聚碳硅烷、硅粉、铝粉、硼粉，混合均匀后得到悬浮液；
将上述步骤(3)中得到的悬浮液加热至80℃～120℃，进行蒸发，直到溶剂完全挥发，得到块状混合物，将块状混合物研磨，过200目以下的筛,得到混合粉末；
将上述步骤(1)中得到的分散后的短切碳纤维和上述步骤(4)中得到的混合粉末捣碎、混合，得混合均匀的泥浆；
将上述步骤(5)中得到混合均匀的泥浆置于石墨模具中进行冷压定型，再置于真空热压炉中，在氩气气氛中，加热至300℃，再以1～５℃/min的升温速度，压力为12.4MPa．加热至300℃～1000℃，并且在压力为26.5MPa、温度为1000℃～1900℃下恒温2～4h进行热压烧结，烧结后，自然降温至室温，制得碳纤维增强碳化硅（Csf/C-SiC）复合材料。
2.根据权利要求1所述的碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其特征在于，上述步骤(1)中所述的碳纤维为聚丙烯氰基碳纤维、沥青基碳纤维中的一种或几种。
3.根据权利要求1所述的碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其特征在于，上述步骤(2)中所述的碳纤维的体积分数为40vol%-60vol%，强力分散后短纤维长度为1mm-5mm。
4.根据权利要求1所述的碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法，其特征在于，上述步骤(3)中所述的有机溶剂为正己烷、二甲苯中的一种。
CN201610277281.4A 2016-05-01 2016-05-01 碳纤维增强碳化硅（Csf/C-SiC）复合材料的制备方法 Pending CN105967712A (zh)

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CN106582521A (zh) * 2016-12-17 2017-04-26 牟燕蓉 碳化硅‑沥青炭吸附粒的制备方法
CN106582521B (zh) * 2016-12-17 2019-02-05 河北亚鼎新材料科技有限公司 碳化硅-沥青炭吸附粒的制备方法
CN108101542A (zh) * 2017-12-07 2018-06-01 南京航空航天大学 一种SiC泡沫及其制备方法
RU2718682C2 (ru) * 2018-09-12 2020-04-13 Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) Способ изготовления керамики на основе карбида кремния, армированного волокнами карбида кремния
CN109437955A (zh) * 2018-12-13 2019-03-08 上海康碳复合材料科技有限公司 一种基于聚碳硅烷改性的刹车材料快速制备方法
CN109437955B (zh) * 2018-12-13 2021-06-29 上海康碳复合材料科技有限公司 一种基于聚碳硅烷改性的刹车材料快速制备方法
CN112191725A (zh) * 2020-09-29 2021-01-08 马鞍山市凯通新能源科技有限公司 新能源汽车电池盒的压制工艺
CN112552063A (zh) * 2020-12-25 2021-03-26 长沙三泰新材料有限公司 一种碳纤维增强碳化硅复合材料的制备方法

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