CN112279663A - 一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法 - Google Patents

一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法 Download PDF

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CN112279663A
CN112279663A CN202011176983.6A CN202011176983A CN112279663A CN 112279663 A CN112279663 A CN 112279663A CN 202011176983 A CN202011176983 A CN 202011176983A CN 112279663 A CN112279663 A CN 112279663A
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fiber reinforced
matrix composite
composite material
ceramic matrix
continuous
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CN112279663B (zh
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姜娟
倪娜
赵晓峰
丁奇
肖巍伟
史银春
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Shanghai Jiaotong University
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Abstract

本发明涉及一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括首先将连续陶瓷纤维预制体置于模具中，随后将纳米陶瓷粉体少量多次逐步倒入模具中连续陶瓷纤维预制体上，并经过机械振荡使纳米陶瓷粉体充分填充预制体内部的孔隙；之后将所得松散复合材料采用一定压力进行压制成型，得到坯体；然后将坯体置于闪烧炉中，升温至预设温度，并施加预设电场强度的电场，直至出现闪烧现象；随后将电源由恒压状态转变为恒流状态，并在预设电流密度下保温一段时间，最后经降温冷却后即得到连续纤维增强陶瓷基复合材料。与现有技术相比，本发明具有烧结温度低、制备周期短、所得复合材料更加致密、陶瓷晶粒更细小、力学性能更加优异等优点。

Description

一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法
技术领域
本发明属于连续纤维增强陶瓷基复合材料技术领域，涉及一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法。
背景技术
连续纤维增强陶瓷基复合材料是将连续陶瓷纤维植入陶瓷基体中形成的一种高性能复合材料。连续纤维增强陶瓷基复合材料不仅具有陶瓷基体耐高温、抗氧化、抗蠕变、高强度、耐腐蚀等优点，还可以克服块体结构陶瓷断裂韧性低和抗冲击性能差的缺点，其假塑性断裂模式可以避免使用过程中结构件脆性断裂引起的灾难性问题。连续纤维增强陶瓷基复合材料作为一种综合性能优异的高温热结构材料，在航空、航天和核能领域具有广泛的应用前景(Rebecca Gottlieb,Shannon Poges,Chris Monteleone,Steven L Suib,Continuous fiber-reinforced ceramic matrix composites,In book:AdvancedCeramic Materials,2016Scrivener Publishing LLC.)。
目前制备连续纤维增强陶瓷基复合材料的方法主要有：(1)气相法，主要指化学气相渗透法(Chemical Vapor Infiltration:CVI)；(2)液相法，主要包括先驱体转化法(Polymer Infiltration and Pyrolysis:PIP)和溶胶-凝胶法(Sol-gel)；(3)固相法，即热压烧结法(Hot Press Sintering:HPS)。化学气相渗透技术采用气相先驱体高温裂解，在纤维表面沉积获得陶瓷基复合材料。这种方法制备的复合材料中纤维损伤较小，但是沉积速度慢，制备周期长，一般需要数月的时间才能获得最终的复合材料，制备成本很高，制备的复合材料孔隙率高(～15％)(R.Naslain,F.Langlais,R.Fedou,The CVI processing ofceramic matrix composites,Journal of Physique Colloques,1989,50(C5):191-207.)。液相法中，先驱体转换法和溶胶-凝胶法是用先驱体或者溶胶浸渍到纤维预制体内部，通过高温裂解陶瓷化生成陶瓷基体，从而得到陶瓷复合材料。这种方法热处理温度较低，但是陶瓷收率低，一般需要多次浸渍，所以数周的制造周期，且得到的复合材料也不可避免的含有～10％的孔隙率(G.Motz,S.Schmidt,S.Beyer,The PIP process:precursorproperties and applications,in Ceramic Matrix Composites:Fiber ReinforcedCeramics and their Applications,2008Wiley-VCH Verlag GmbH&Co.KGaA.4.E.Rodeghiero,B.Moore,B.Wolkenberg,M.Wuthenow,O.Tse,E.Giannelis,Sol-gel synthesis of ceramic matrix composites,Materials Science and Engineering:A,1998,244(1):11-21.)。热压烧结法是首先将纤维浸渍在含有基体粉料的浆料中，然后将浸有浆料的纤维制成无纬布，层叠后热压烧结制得复合材料。这种方法制备简单，但是纤维同时在高温高压下处理会受到严重损伤，从而使纤维增韧作用大大减弱(K.Keller,G.Jefferson,R.Kerans,Oxide-Oxide composites,In:Handbook of CeramicComposites.2005Springer.)。
发明内容
本发明的目的就是提供一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，用于解决现有连续纤维增强陶瓷基复合材料制备温度高、制备时间长、制备工艺繁琐的技术问题。
本发明的目的可以通过以下技术方案来实现：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)将连续陶瓷纤维预制体裁成模具大小，然后将其置于模具中，随后将纳米陶瓷粉体少量多次逐步倒入模具中连续陶瓷纤维预制体上，并经过机械振荡使纳米陶瓷粉体充分填充预制体内部的孔隙；之后将所得松散复合材料采用一定压力进行压制成型，得到坯体；
2)将坯体置于闪烧炉中，升温至预设温度，并施加预设电场强度的电场，直至出现闪烧现象；
3)闪烧开始后，将电源由恒压状态转变为恒流状态，并在预设电流密度下保温一段时间，最后经降温冷却后即得到连续纤维增强陶瓷基复合材料。
进一步地，步骤1)中，连续陶瓷纤维包括SiC纤维、Al2O3纤维及ZrO2纤维中的至少一种。
进一步地，步骤1)中，预制体结构包括二维纤维布叠层、三维针刺或2.5维编织预制体，模具中连续陶瓷纤维预制体的体积分数为30-40％。连续陶瓷纤维预制体是用纤维编织而成，其间充斥着大量孔隙，预制体中纤维所占体积分数为30-40％。步骤1)中将预制体裁成模具大小，之后加入的粉体即填充于纤维之间的孔隙中。
进一步地，步骤1)中，所述的纳米陶瓷粉体包括SiC粉、Al2O3粉或ZrO2粉中的至少一种；粉体尺寸为50-500nm。
进一步地，步骤1)中，所述的机械振荡时间为20-120min；
所述的压制成型中，成型压力为100-300MPa，成型时间为60-600s。
进一步地，步骤2)中，所述的坯体形状为长条形或圆柱形，坯体在电场方向的长度为1-30cm。
进一步地，步骤2)中，升温速率为2-20℃/min，预设温度为0.3Tm-0.8Tm，其中Tm为纳米陶瓷粉体的熔融温度，达到预设温度后进入保温状态。
进一步地，步骤2)中，所述的预设电场强度为20-1000V/cm。
进一步地，步骤3)中，所述的恒流状态下，电流密度为10-500mA/mm2。
进一步地，步骤3)中，所述的冷却包括：以5-30℃/min的降温速率冷却到室温。
与现有技术相比，本发明将闪烧技术应用于连续纤维增强陶瓷基复合材料的制备，仅需要几个小时的时间，即可获得陶瓷基复合材料。相对传统制备方法，利用闪烧技术制备陶瓷基复合材料所需设备非常简单，烧结温度较低，制备周期大大缩短，所获得的复合材料更加致密，陶瓷晶粒更细小，材料的力学性能更加优异。
附图说明
图1为实施例1中制备得到的SiC纤维/SiC陶瓷复合材料的扫描电镜图。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)将二维纤维布叠层、三维针刺或2.5维编织的SiC纤维、Al2O3纤维或ZrO2纤维作为连续陶瓷纤维预制体，裁成模具大小并置于长度为1-30cm的长条形或圆柱形模具中，其中纤维体积分数为30-40％。随后将粒径为50-500nm的SiC、Al2O3或ZrO2纳米陶瓷粉体少量多次逐步倒入模具中的连续陶瓷纤维预制体上，并经过20-120min机械振荡使纳米陶瓷粉体充分填充预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以100-300MPa的成型压力压制60-600s，得到坯体；
3)将坯体置于闪烧炉中，以2-20℃/min的升温速率加热至预设温度0.3Tm-0.8Tm(Tm为纳米陶瓷粉体的熔融温度)，之后保温20-120min；
4)对坯体长度方向上的两端施加预设电场强度(20-1000V/cm)的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在预设电流密度(10-500mA/mm2)下保温1-30min，最后以5-30℃/min的降温速率冷却到室温，即得到连续纤维增强陶瓷基复合材料。
以下实施例以本发明技术方案为前提进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)在2cm×10cm×2cm的长条形模具中，加入模具大小体积分数40％的三维针刺SiC纤维预制体，随后将粒径为300nm的SiC粉体分5次倒入模具中的SiC纤维预制体上，并经过30min机械振荡使SiC粉体充分填充SiC纤维预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以200MPa的成型压力压制120s，得到坯体；
3)将坯体置于闪烧炉中，以5℃/min的升温速率加热至预设温度1300℃，并保温30min；
4)对坯体长度方向上的两端施加预设电场强度为100V/cm的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在200mA/mm2的预设电流密度下保温10min，最后以5℃/min的降温速率冷却到室温，即得到SiC纤维/SiC陶瓷复合材料。
如图1所示为本实施例所制备的SiC纤维/SiC陶瓷复合材料的SEM图，从图中可以看出，所得复合材料中基体分布均匀，致密度高达97％，且纤维和界面具有较好的结合性。所得复合材料的拉伸强度可达280MPa，高于常规PIP方法制备SiC纤维/SiC复合材料的强度(约200MPa)。
实施例2：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)在4cm×10cm×2cm的长条形模具中，加入模具大小体积分数30％的二维纤维布叠层SiC纤维预制体，随后将粒径为200nm的SiC粉体分8次逐步倒入模具中的SiC纤维预制体上，并经过120min机械振荡使SiC粉体充分填充SiC纤维预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以200MPa的成型压力压制240s，得到坯体；
3)将坯体置于闪烧炉中，以10℃/min的升温速率加热至预设温度1250℃，之后保温30min；
4)对坯体长度方向上的两端施加预设电场强度为200V/cm的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在300mA/mm2的预设电流密度下保温10min，最后以10℃/min的降温速率冷却到室温，即得到SiC纤维/SiC陶瓷复合材料。所得复合材料的拉伸强度可达248MPa，高于常规PIP方法制备SiC纤维/SiC复合材料的强度(约200MPa)。
实施例3：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)在2cm×10cm×5cm的长条形模具中，加入模具大小体积分数35％的2.5维SiC纤维预制体，随后将粒径为150nm的SiC粉体少量多次逐步倒入模具中的SiC纤维预制体上，并经过60min机械振荡使SiC粉体充分填充SiC纤维预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以300MPa的成型压力压制300s，得到坯体；
3)将坯体置于闪烧炉中，以2℃/min的升温速率加热至预设温度1300℃，之后保温20min；
4)对坯体长度方向上的两端施加预设电场强度为500V/cm的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在200mA/mm2的预设电流密度下保温15min，最后以10℃/min的降温速率冷却到室温，即得到SiC纤维/SiC陶瓷复合材料。所得复合材料的拉伸强度可达265MPa，高于常规PIP方法制备SiC纤维/SiC复合材料的强度(约200MPa)。
实施例4：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)在
Figure BDA0002748966530000051
的圆柱形模具中，加入模具大小体积分数30％的二维纤维布叠层Al2O3纤维预制体，随后将粒径为250nm的Al2O3粉体分10次倒入模具中的Al2O3纤维预制体上，并经过60min机械振荡使Al2O3粉体充分填充Al2O3纤维预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以150MPa的成型压力压制300s，得到坯体；
3)将坯体置于闪烧炉中，以10℃/min的升温速率加热至预设温度1100℃，之后保温60min；
4)对坯体长度方向上的两端施加预设电场强度为1000V/cm的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在50mA/mm2的预设电流密度下保温10min，最后以10℃/min的降温速率冷却到室温，即得到Al2O3纤维/Al2O3陶瓷复合材料。所得复合材料的拉伸强度可达239MPa。
实施例5：
一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，包括以下步骤：
1)在
Figure BDA0002748966530000061
的圆柱形模具中，加入模具大小体积分数30％的二维纤维布叠层ZrO2纤维预制体，随后将粒径为500nm的ZrO2粉体分6次倒入模具中的ZrO2纤维预制体上，并经过120min机械振荡使ZrO2粉体充分填充ZrO2纤维预制体内部的孔隙，得到松散复合材料；
2)将松散复合材料以250MPa的成型压力压制600s，得到坯体；
3)将坯体置于闪烧炉中，以10℃/min的升温速率加热至预设温度950℃，之后保温30min；
4)对坯体长度方向上的两端施加预设电场强度为1000V/cm的电场，直至出现闪烧现象，之后将电源由恒压状态转变为恒流状态，并在50mA/mm2的预设电流密度下保温15min，最后以15℃/min的降温速率冷却到室温，即得到ZrO2纤维/ZrO2陶瓷复合材料。所得复合材料的拉伸强度可达233MPa。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

1.一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，该方法包括以下步骤：
1)将连续陶瓷纤维预制体置于模具中，加入纳米陶瓷粉体，并依次经过机械振荡与压制成型后，得到坯体；
2)将坯体升温至预设温度并施加预设电场强度的电场，直至出现闪烧现象；
3)将电源由恒压状态转变为恒流状态并保温，冷却后即得到连续纤维增强陶瓷基复合材料。
2.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤1)中，连续陶瓷纤维包括SiC纤维、Al2O3纤维及ZrO2纤维中的至少一种。
3.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤1)中，预制体结构包括二维纤维布叠层、三维针刺或2.5维编织预制体，连续陶瓷纤维预制体的体积分数为30-40％。
4.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤1)中，所述的纳米陶瓷粉体包括SiC粉、Al2O3粉或ZrO2粉中的至少一种；粉体尺寸为50-500nm。
5.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤1)中，所述的机械振荡时间为20-120min；
所述的压制成型中，成型压力为100-300MPa，成型时间为60-600s。
6.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤2)中，所述的坯体形状为长条形或圆柱形，坯体在电场方向的长度为1-30cm。
7.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤2)中，升温速率为2-20℃/min，预设温度为0.3Tm-0.8Tm，其中Tm为纳米陶瓷粉体的熔融温度。
8.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤2)中，所述的预设电场强度为20-1000V/cm。
9.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤3)中，所述的恒流状态下，电流密度为10-500mA/mm2。
10.根据权利要求1所述的一种利用闪烧技术制备连续纤维增强陶瓷基复合材料的方法，其特征在于，步骤3)中，所述的冷却包括：以5-30℃/min的降温速率冷却到室温。
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