CN103086731A - 高强度纤维增强陶瓷基复合材料的微区原位反应制备方法 - Google Patents
高强度纤维增强陶瓷基复合材料的微区原位反应制备方法 Download PDFInfo
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Abstract
本发明涉及高强度纤维增强陶瓷基复合材料的微区原位反应制备方法,提供了一种高强度纤维增强陶瓷基复合材料的微区原位反应制备方法,该方法包括以下步骤:(i)在复合材料纤维预制体表面沉积界面层以对纤维增强体进行保护,其中,所述界面层包括PyC界面、BN界面、SiC界面、以及它们的复合界面;所述界面层的厚度为10-2000nm;(ii)向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相,以获得复合材料预成型体;(iii)将所述复合材料预成型体进行致密化处理,获得高强度纤维增强陶瓷基复合材料,其中,所述致密化处理包括高温处理,使得Si3N4与复合材料中的含碳相之间通过相互扩散而发生微区原位反应形成SiC相,其中,所述高温处理的温度为1200-2300℃。
Description
技术领域
本发明属于复合材料领域,涉及一种高强度纤维增强陶瓷基复合材料的微区原位反应制备方法。更具体地说,本发明涉及一种使PIP(polymer infiltration andpyrolysis,有机前驱体浸渍裂解)工艺制备纤维增强陶瓷基复合材料力学性能提高的方法。
背景技术
纤维增强陶瓷基复合材料由于具有低密度、高强度、高韧性、耐高温、抗氧化、非脆性断裂等一系列优点,在航空航天、国防军工、新能源以及交通运输等重要领域具有广泛的应用前景。目前常见的纤维增强陶瓷基复合材料主要包括以碳纤维和碳化硅纤维作为增强体,以碳化硅(SiC)作为基体所制备的碳化硅基复合材料,分别为碳纤维增强碳化硅基复合材料(C/SiC复合材料)和碳化硅纤维增强碳化硅基复合材料(SiC/SiC复合材料)。同时,为满足不同应用领域的使用要求,还包括采用不同组分对复合材料基体进行改性所获得的SiC基复合材料,如添加自愈合相的SiC基复合材料和添加超高温陶瓷相的耐超高温烧蚀Si C基复合材料。
目前,SiC基复合材料的制备方法主要包括CVI法(化学气相渗透法,Chemical Vapor Infiltration)、PIP法、HP法(热压烧结法,hot pressing)、MSI法(熔融硅渗透法,Molten Silicon infiltration)。HP法由于在制备过程中需要承受高温高压,因此目前仅适合于简单形状复合材料的制备。MSI法由于在制备过程不可避免地将残留部分游离硅,将对复合材料的高温性能产生不利的影响,目前该方法主要用于低成本快速制备新型刹车材料。因此,复合材料常用的制备方法目前主要集中在CVI法和PIP法。CVI工艺所制备复合材料基体由相应的源气间发生化学反应原位形成,因此基体间具有非常高的结合强度,所制备的复合材料强度较高,但是CVI工艺存在制备周期长且设备复杂、投资大,同时其副产物具有非常强的腐蚀性等不足。PIP工艺可制备形状复杂的陶瓷基复合材料构件且制备温度低,是目前制备陶瓷基复合材料的一种重要手段。在PIP工艺的有机前驱体裂解过程中,伴随着固体产物密度增加以及有机小分子逸出,发生体积收缩,在复合材料中形成大量的气孔。为获得具有高致密度的陶瓷基复合材料,需要对复合材料进行多次浸渍-裂解循环。由于采用PIP工艺对陶瓷基复合材料进行致密化时,前驱体裂解形成的陶瓷产物主要是对复合材料中存在的孔隙进行填充,无法达到烧结的效果,因此,复合材料不同浸渍裂解循环过程中所形成的陶瓷相之间以及基体和纤维增强体表面界面层之间无法形成强结合,导致采用PIP工艺所制备的复合材料强度较CVI工艺的低。
因此,本领域迫切需要开发出一种提高PIP工艺制备陶瓷基复合材料力学性能的方法,该方法能够克服目前PIP工艺制备纤维增强陶瓷基复合材料因基体结合强度较低而导致复合材料力学性能低的不足。
发明内容
本发明提供了一种新颖的高强度纤维增强陶瓷基复合材料的制备方法,从而解决了现有技术中存在的问题。
本发明提供了一种高强度纤维增强陶瓷基复合材料的微区原位反应制备方法,该方法包括以下步骤:
(i)在复合材料纤维预制体表面沉积界面层以对纤维增强体进行保护,其中,所述界面层包括PyC界面、BN界面、SiC界面、以及它们的复合界面;所述界面层的厚度为10-2000nm;
(ii)向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相,以获得复合材料预成型体;
(iii)将所述复合材料预成型体进行致密化处理,获得高强度纤维增强陶瓷基复合材料,其中,所述致密化过程包括高温处理,使得Si3N4与复合材料中的含碳相之间通过相互扩散而发生微区原位反应形成SiC相,其中,所述高温处理的温度为1200-2300℃。
在一个优选的实施方式中,在所述步骤(ii)中,向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相采用浸渍工艺和/或化学气相渗透工艺进行,其中,
所述浸渍工艺包括:
将陶瓷粉体和/或有机前驱体溶液在溶剂中混合获得均匀的浆料,其中,所述陶瓷粉体包括Si3N4、SiC、ZrB2、ZrC、HfC、HfB2、BN和B4C中的一种或多种;所述有机前驱体溶液包括碳前驱体、SiC前驱体、Si3N4前驱体、BN前驱体、ZrC前驱体、ZrB2前驱体以及它们的混合物;并且所得的浆料中含有Si3N4粉体或Si3N4前驱体中的至少一种;
将所述复合材料纤维预制体在所得的浆料中进行浸渍,使浆料渗透入纤维预制体的孔隙中;以及
将浸渍浆料后的复合材料预制体进行干燥并裂解,获得含Si3N4陶瓷相的复合材料预成型体;
所述化学气相渗透工艺包括:
将所述纤维预制体置于化学气相沉积炉中,抽真空并升温至900-1350℃的沉积温度;以及
向炉膛中充入硅的气态前驱体和氮的气态前驱体,使它们在800-1350℃的温度下发生裂解并在纤维预制体的表面形成Si3N4陶瓷相。
在另一个优选的实施方式中,所述高温处理的时间为1分钟-10小时,粗粒环境为非氧化环境。
在另一个优选的实施方式中,所述致密化处理使用PIP工艺或者包含PIP工艺的复合工艺进行,循环次数为1-25次。
在另一个优选的实施方式中,所述复合材料纤维预制体包括短纤维、一维无纬布、二维纤维布、立体纤维编制体;所述纤维增强体包括碳纤维、SiC纤维、Si3N4纤维。
在另一个优选的实施方式中,所述Si3N4陶瓷相使用平均粒径为10-5000nm的Si3N4颗粒。
在另一个优选的实施方式中,所述界面层为PyC界面。
在另一个优选的实施方式中,所述界面层的厚度为50-400nm。
在另一个优选的实施方式中,所述高温处理的温度为1400-1650℃。
附图说明
图1示出了根据本申请实施例1的高温处理前后C/SiC-Si3N4复合材料的XRD(X射线衍射)图谱。如图1所示,通过比较XRD图谱可以发现,在处理过程中复合材料中的Si3N4相的衍射峰得到明显的减弱,而SiC的衍射峰得到了明显的加强,说明Si3N4在高温下发生反应转化为了SiC。
图2示出了根据本申请实施例1的C/SiC-Si3N4复合材料断面SEM(扫描电子显微镜)图片。复合材料断面具有明显的拔出纤维,说明采用本发明所述方法未改变纤维增强陶瓷基复合材料的基本特性。
图3示出了根据本申请实施例1的不同PIP工艺制备的C/SiC复合材料抛光面表面形貌。如图3所示,(a)未引入Si3N4相,基体结合力差,部分基体在抛光时被剥落;(b)引入了Si3N4相,基体结合强度提高,抛光面平整。
图4示出了根据本申请实施例1的高温处理后的C/SiC-Si3N4复合材料断面高倍SEM形貌。如图4所示,所拔出纤维具有比较粗糙的表面,说明在微区原位反应过程中纤维表面的PyC界面层与基体间发生了化学反应,从而提高了纤维增强体和界面的结合强度。
具体实施方式
本发明的发明人在经过了广泛而深入的研究之后发现,通过在PIP工艺制备陶瓷基复合材料致密化过程中,利用基体中不同组分间以及基体与纤维增强体表面界面层间发生微区原位化学反应,形成原位结合相,能够提高复合材料基体以及基体与纤维增强体界面间的结合强度,从而使复合材料的力学性能得到提高。基于上述发现,本发明得以完成。
本发明的技术构思如下:
针对PIP工艺制备碳化硅基复合材料基体结合强度低的特点,在基体中引入微区原位反应,提高有机前驱体裂解固体产物间的结合强度,提高复合材料承受载荷的能力;在该工艺中首先通过向复合材料基体中引入Si3N4陶瓷相,利用高温条件下Si3N4与复合材料基体中的游离碳和裂解碳界面层之间发生微观尺度的原位反应生成SiC;由于原位生成的SiC相能够提高复合材料基体以及复合材料基体与纤维表面界面层之间的结合强度,因此复合材料的力学强度能够得到大幅度的提高。
本发明的制备高强度纤维增强陶瓷基复合材料的方法包括以下步骤:
(i)在复合材料纤维预制体表面沉积界面层以对纤维增强体进行保护;
(ii)向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相,以获得复合材料预成型体;
(iii)将所得的预成型体进行致密化处理,获得具有高致密度的陶瓷基复合材料。
在本发明中,所沉积的界面层包括PyC界面、BN界面、SiC界面以及由上述界面组合形成的复合界面;所述界面层的厚度为10-2000nm,优选50nm-400nm;为提高复合材料基体与纤维表面界面层的结合强度,本发明优选界面层的最外层为PyC界面层。
在本发明中,采用的复合材料纤维预制体包括短纤维、一维无纬布、二维纤维布、立体纤维编制体(2.5D纤维预成型体、三维四向编制体、三维五向编制体、三维针刺纤维预制体);采用的纤维增强体优选碳纤维、SiC纤维和Si3N4纤维。
在本发明中,向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相的方式包括浸渍工艺和/或CVI工艺。当采用浸渍工艺引入Si3N4陶瓷相时,首先将陶瓷粉体和/或有机前驱体溶液在溶剂中混合以获得均匀的浆料,其中,所述陶瓷粉体优选Si3N4、SiC、ZrB2、ZrC、HfC、HfB2、BN和B4C中的一种或多种;所述有机前驱体溶液优选碳前驱体、SiC前驱体、Si3N4前驱体、BN前驱体、ZrC前驱体、ZrB2前驱体以及上述前驱体的混合物;并且所述浆料中含有Si3N4粉体或Si3N4前驱体中的至少一种;接着将所述复合材料纤维预制体在所得的浆料中进行浸渍,使浆料渗透入纤维预制体的孔隙中;然后将浸渍浆料后的复合材料预制体进行干燥并裂解,获得含Si3N4陶瓷相的复合材料预成型体;当采用CVI工艺引入Si3N4陶瓷相时,先将所述纤维预制体置于化学气相沉积炉中,抽真空并升温至沉积温度,随后向炉膛中充入硅的气态前驱体和氮的气态前驱体,使它们在高温下发生裂解并在纤维预制体的内部孔隙中形成Si3N4陶瓷相。
在本发明中,复合材料的致密化方法可以包括PIP工艺或PIP工艺与其他工艺结合的复合工艺,优选PIP工艺。其中,PIP循环次数为1-25次,优选3-15次;有机前驱体裂解温度为500-1600℃,优选800-1200℃;有机前驱体裂解过程升温速度为0.1-50℃/分钟,优选0.5-10℃/分钟;裂解时间为1分钟-10小时,优选30分钟-2小时;裂解环境为非氧化环境,优选Ar气气氛;在PIP工艺过程中可在裂解前对前驱体进行固化处理;PIP致密化所采用的有机前驱体优选SiC前驱体、BN前驱体、ZrC前驱体、ZrB2前驱体以及上述前驱体的混合物;根据复合材料的致密化行为,在致密化过程中对复合材料进行高温处理,使复合材料中的Si3N4陶瓷相和碳相之间发生反应微区原位形成SiC相,其中高温处理温度为1200-2300℃,优选1400-1650℃;高温处理时间为1分钟-10小时,优选30分钟-3小时;高温处理气氛为非氧化气氛,优选Ar气氛或真空。
较佳地,本发明的制备高强度纤维增强陶瓷基复合材料的方法包括以下步骤:
(1)沉积界面:利用CVI技术在纤维预制体表面沉积厚度为100-500nm的裂解碳(PyC);
(2)配制前驱体(PCS)溶液:将聚碳硅烷、氮化硅、二乙烯基苯(DVB)按照质量比=1∶(0.2~1)∶(0.2~0.6),通过湿法球磨,制备均匀分散的含Si3N4颗粒浆料;或者将一定配比的聚碳硅烷、二乙烯基苯和二甲苯通过超声溶解配成澄清PCS溶液;
(3)真空浸渍:将沉积界面后的纤维预制体置于容器中,引入含Si3N4的浆料并真空浸渍;
(4)固化交联:将浸渍后的纤维预制体取出后晾干,在烘箱内120-150℃下保温一段时间;
(5)裂解:将固化后的纤维预制体在900℃下的Ar气氛中进行裂解,裂解时间为0.5小时;
(6)高温处理:将裂解后的复合材料进行1400℃-1650℃的高温处理,处理时间0.1~2小时,处理气氛为氮气或者氩气;
(7)致密化:反复采用PCS溶液进行浸渍与裂解致密化,直至预制体的质量变化小于1%时,完成复合材料的制备。
较佳地,所述氮化硅原料颗粒的平均粒径为50~1000nm。
较佳地,在高温处理在1个周期或者多个周期后,在氮气或氩气气氛保护下,以5~10℃/分钟的升温速率至1400~1650℃下保温10~120分钟。
本发明的制备方法可用于提高复合材料界面与基体间的结合力,并且,作为复合制备手段,可应用于其他陶瓷基复合材料中,如含自愈合相的碳化硅基复合材料(C/SiC-BN、C/SiC-MoSi2、C/SiC-B4C、C/SiC-SiB4等)和含超高温陶瓷相的耐超高温烧蚀碳化硅基体复合材料(如C/SiC-ZB2、C/SiC-ZrC、C/SiC-HfC等)。
本发明的主要优点在于:
本发明在采用PIP工艺制备陶瓷基复合材料的过程中,通过向复合材料中引入部分Si3N4陶瓷相,利用Si3N4在高温条件下与复合材料中的含碳相(基体中的游离碳和PyC界面层)之间发生反应,微区原位形成SiC相,使PIP工艺获得的复合材料基体颗粒以及复合材料基体与纤维表面界面层之间结合强度得到提高,最终获得力学性能优异的纤维增强陶瓷基复合材料。通过采用本发明的方法,在保证PIP工艺制备复合材料优点的同时可使PIP工艺制备复合材料力学性能与CVI工艺制备复合材料力学性能相当;复合材料的力学强度能够得到大幅度的提高;通过本发明的实施可使复合材料的三点弯曲强度由254MPa上升到484MPa。
实施例
下面结合具体的实施例进一步阐述本发明。但是,应该明白,这些实施例仅用于说明本发明而不构成对本发明范围的限制。下列实施例中未注明具体条件的试验方法,通常按照常规条件,或按照制造厂商所建议的条件。除非另有说明,所有的百分比和份数按重量计。
实施例1
将聚碳硅烷、氮化硅、二乙烯基苯按质量比(1∶0.5∶0.5)混合,以二甲苯为溶剂,通过湿法球磨24小时形成分散均匀的浆料。将沉积有厚度约150nmPyC界面层的三维针刺碳纤维预制体在上述浆料中进行真空浸渍使浆料渗透到纤维预制体孔隙中,浸渍时间为6小时。将浸渍后的纤维预制体干燥后在120℃的Ar气氛中固化6小时后以3℃/分钟的速率升温到900℃进行裂解获得复合材料预成型体,保温时间为1小时。将复合材料纤维预成型体在Ar气氛下1600℃保温1小时,使Si3N4和PCS裂解碳以及PyC界面之间发生微区原位反应。随后以PCS作为前驱体,采用PIP工艺对复合材料进行致密化处理直至经一次PIP循环后样品增重率小于1%完成复合材料致密化。由图1,C/SiC-Si3N4复合材料XRD图谱,可知,未经过高温处理的C/SiC-Si3N4复合材料存在明显的α-Si3N4,高温处理后Si3N4与无定型碳反应,Si3N4含量降低,无定型SiC开始结晶。由图2可知,基体间结合紧密,有纤维拔出现象,长度较短,具有明显的纤维增强陶瓷基复合材料特征。由图3中对比发现,引入Si3N4相高温处理后,基体结合强度提高,基体抛光面致密并且平整。由图4可知,拔出纤维表面比较粗糙,说明在界面处Si3N4相与界面层发生化学反应,增强了界面间的结合力。通过该工艺制备的三维针刺C/SiC三点抗弯平均强度为484MPa,力学性能明显提高。
实施例2
按照实施例1,在形成复合材料预成型体后采用聚碳硅烷与二乙烯基苯(质量比为1∶0.5)的二甲苯溶液进行2次PIP循环后再进行高温微区原位反应。随后以PCS为前驱体通过PIP工艺对复合材料进行致密化。通过该工艺制备的三维针刺C/SiC三点抗弯强度为448MPa。由于引入通过2次PIP循环后,在复合材料基体中引入了更多的碳源,减少了界面层与Si3N4相之间的反应程度,使得结合界面较直接高温反应时稍弱,所得复合材料强度稍低使纤维拔出明显,拔出长度较长。
实施例3
按照实施例1,将样品放置于真空碳管炉内氮气气氛保护1700℃并保温2小时。然后,利用PCS作为前驱体,采用PIP工艺对复合材料进行致密化处理直至经一次PIP循环后样品增重率小于1%完成复合材料致密化。测得其抗弯强度为393MPa。力学性能较传统PIP功能所制备复合材料强度仍有改进,但由于高温处理温度温度较高且时间较长,可能导致纤维增强体强度发生退化,从而导致复合材料强度有所降低。
对比例1
按照实施例1,将聚碳硅烷、氮化硅、二乙烯基苯按质量比(1∶0.5∶0.5)混合,以二甲苯为溶剂,通过湿法球磨24小时形成分散均匀的浆料。将沉积有厚度约150nm PyC界面层的三维针刺碳纤维预制体在上述浆料中进行真空浸渍使浆料渗透到纤维预制体孔隙中,浸渍时间为6小时。将浸渍后的纤维预制体干燥后在120℃的Ar气氛中固化6小时后以3℃/分钟的速率升温到900℃进行裂解获得复合材料预成型体,保温时间为1小时。随后以PCS作为前驱体,采用PIP工艺对复合材料进行致密化处理直至经一次PIP循环后样品增重率小于1%完成复合材料致密化。测得其抗弯强度为383MPa。引入Si3N4相一定程度上提高了复合材料的强度。但未经高温处理,纤维与基体间仍为弱界面结合,纤维拔出长,力学性能低于实施例1中的最优制备方式。
对比例2
利用传统PIP方式制备复合材料,采用PIP工艺对复合材料进行致密化处理直至经一次PIP循环后样品增重率小于1%完成复合材料致密化。测得其抗弯强度为254MPa。基体间结合较差,纤维拔出长,纤维与基体间为弱结合,力学性能远低于实施例1中的最优制备方式。
在本发明提及的所有文献都在本申请中引用作为参考,就如同每一篇文献被单独引用作为参考那样。此外应理解,在阅读了本发明的上述讲授内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
Claims (9)
1.一种高强度纤维增强陶瓷基复合材料的微区原位反应制备方法,该方法包括以下步骤:
(i)在复合材料纤维预制体表面沉积界面层以对纤维增强体进行保护,其中,所述界面层包括PyC界面、BN界面、SiC界面、以及它们的复合界面;所述界面层的厚度为10-2000nm;
(ii)向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相,以获得复合材料预成型体;
(iii)将所述复合材料预成型体进行致密化处理,获得高强度纤维增强陶瓷基复合材料,其中,所述致密化处理包括高温处理,使得Si3N4与复合材料中的含碳相之间通过相互扩散而发生微区原位反应形成SiC相,其中,所述高温处理的温度为1200-2300℃。
2.如权利要求1所述的方法,其特征在于,在所述步骤(ii)中,向所述复合材料纤维预制体的孔隙中引入Si3N4陶瓷相采用浸渍工艺和/或化学气相渗透工艺进行,其中,
所述浸渍工艺包括:
将陶瓷粉体和/或有机前驱体溶液在溶剂中混合获得均匀的浆料,其中,所述陶瓷粉体包括Si3N4、SiC、ZrB2、ZrC、HfC、HfB2、BN和B4C中的一种或多种;所述有机前驱体溶液包括碳前驱体、SiC前驱体、Si3N4前驱体、BN前驱体、ZrC前驱体、ZrB2前驱体、以及它们的混合物;并且所得的浆料中含有Si3N4粉体或Si3N4前驱体中的至少一种;
将所述复合材料纤维预制体在所得的浆料中进行浸渍,使浆料渗透入纤维预制体的孔隙中;以及
将浸渍浆料后的复合材料预制体进行干燥并裂解,获得含Si3N4陶瓷相的复合材料预成型体;
所述化学气相渗透工艺包括:
将所述纤维预制体置于化学气相沉积炉中,抽真空并升温至900-1350℃的沉积温度;以及
向炉膛中充入硅的气态前驱体和氮的气态前驱体,使它们在800-1350℃的温度下发生裂解并在纤维预制体的表面形成Si3N4陶瓷相。
3.如权利要求1或2所述的方法,其特征在于,所述高温处理的时间为1分钟-10小时,环境为非氧化性环境。
4.如权利要求1或2所述的方法,其特征在于,所述致密化处理使用PIP工艺或者包含PIP工艺的复合工艺进行,循环次数为1-25次。
5.如权利要求1或2所述的方法,其特征在于,所述复合材料纤维预制体包括短纤维、一维无纬布、二维纤维布、立体纤维编制体;所述纤维增强体包括碳纤维、SiC纤维、Si3N4纤维。
6.如权利要求1或2所述的方法,其特征在于,所述Si3N4陶瓷相使用平均粒径为10-5000nm的Si3N4颗粒。
7.如权利要求1或2所述的方法,其特征在于,所述界面层为PyC界面。
8.如权利要求1或2所述的方法,其特征在于,所述界面层的厚度为50-400nm。
9.如权利要求1或2所述的方法,其特征在于,所述高温处理的温度为1400-1650℃。
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