CN110563467B - 一种低温SiC纤维表面石墨界面的制备方法 - Google Patents

一种低温SiC纤维表面石墨界面的制备方法 Download PDF

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CN110563467B
CN110563467B CN201910971091.6A CN201910971091A CN110563467B CN 110563467 B CN110563467 B CN 110563467B CN 201910971091 A CN201910971091 A CN 201910971091A CN 110563467 B CN110563467 B CN 110563467B
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王一光
陶鹏飞
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Beijing Institute of Technology BIT
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Abstract

本发明涉及一种低温SiC纤维表面石墨界面的制备方法，属于核燃料包壳管制备领域。本发明的目的是为了解决现有制备SiCf/SiC复合材料采用的PyC界面在高剂量中子辐照后，界面发生退化，界面处产生裂缝，导致材料力学性能和导热性能降低等问题，提供一种低温SiC纤维表面石墨界面的制备方法；该方法首先在SiC纤维预制体表面沉积PyC界面，然后通过强磁场及加热实现PyC界面的石墨化，在维持SiC纤维原有力学性能的同时提高SiCf/SiC复合材料的高温抗中子辐照能力。本发明利用强磁场辅助加热使PyC界面石墨化，降低石墨化温度，可避免高温加热对SiC纤维的损伤，防止SiC纤维晶粒长大，保持SiC纤维力学强度，也会保证SiCf/SiC复合材料的力学性能。

Description

一种低温SiC纤维表面石墨界面的制备方法
技术领域
本发明涉及一种低温SiC纤维表面石墨界面的制备方法，属于核燃料包壳管制备领域。
背景技术
对于SiCf/SiC复合材料，界面相理论上应采用具有各项异性的、层状结构的石墨，以达到偏转裂纹的效果。石墨层间以范德华力结合，当裂纹尖端扩展与其相遇时，会在弱结合的原子层之间发生偏转，从而使SiCf/SiC材料呈现非线性断裂。但是在界面相实际制备中，常使用热解碳(PyC)界面代替石墨，现有的采用化学气相渗透法(CVI)制备的核级SiCf/SiC材料多采用单层PyC或多层PyC/SiC作为材料界面层，界面层厚度通常为20～500nm。PyC界面通常以气态碳氢化合物作为前体，通过化学气相沉积(CVD)工艺沉积在纤维预制体表面。尽管PyC具有较小的中子吸收截面，但是作为核级SiCf/SiC复合材料的界面已被证明在高剂量中子辐照条件下，PyC界面会受到严重的辐射损伤，使得SiCf/SiC复合材料难以保持优异的机械性能和断裂韧性。例如，Nozawa等通过纤维顶出实验(Push-out test)研究了中子辐照(1073K，7.7dpa)对分别具有单层PyC及多层(PyC/SiC)n界面相的CVI Hi-NicalonType S SiCf/SiC复合材料界面剪切强度的影响规律，发现了辐照后SiCf/(PyC/SiC)n/SiC复合材料界面剪切强度下降幅度大于SiCf/PyC/SiC复合材料。Ozawa等分别研究了FCVITSA3SiCf/SiC和HNLS SiCf/SiC复合材料在辐照温度为740～750℃、中子通量分别为3.1×1025n/m2及1.2×1026n/m2时的力学性能变化规律。结果表明：复合材料纤维/基体界面滑移应力均显著下降。Katoh和Bergquist等研究了辐照温度为300℃、500℃及800℃，辐照剂量为71～74dpa时，CVI Hi-Nicalon Type S SiCf/SiC复合材料的微观结构及宏观性能变化：发现复合材料PyC界面处产生裂缝，界面结合强度降低，力学性能呈不同程度下降。Koyanagi和Nozawa等研究了辐照导致的CVI SiCf/SiC复合材料机械性能衰退机理，当辐照剂量为100dpa、辐照温度为319℃和629℃时，复合材料PyC界面结合强度分别变强及变弱，导致前者呈脆性断裂、后者断口有大量纤维拔出，材料强度均大幅下降。现有的结果表明在经高剂量(>70dpa)中子辐照后PyC退化，由乱层石墨结构演变为高度富碳的无定形C/Si混合物，界面相性能衰退，产生应力，引起界面脱粘，进而影响SiCf/SiC复合材料在高剂量中子辐照环境下的力学及导热性能。
上述采用化学气相沉积法制备的PyC界面，均为具有一定取向的、非连续的“类石墨烯”结构，为“短程有序”状态，因此具有一定的导电性，能对磁场的作用做出一定的响应。经强磁场处理后，“类石墨烯”结构会沿磁场方向取向，堆叠成的纳米石墨片层与磁场方向平行，从而使PyC发生石墨化转变。
而石墨具有较高的散射截面和极低的热中子吸收截面，其抗辐照性能极好，常作为高温气冷堆的支撑体首选材料，且相比于PyC，石墨材料的导热性能也更为优异。与此同时，石墨为层状结构结晶度高，作为SiCf/SiC复合材料界面能得到良好的裂纹偏转效果。一般来说，通过1600℃以上高温热处理可以实现PyC材料的石墨化，但1500℃以上的高温会引起SiC纤维中的晶粒长大，从而导致SiC纤维的力学性能下降。而若将石墨作为SiCf/SiC复合材料的界面层，需解决以下问题：一、降低PyC材料石墨化的温度(不高于1300℃)，以免损坏SiC纤维的力学，保证纤维化学性能不变；二、防止界面层氧化，保证界面层的完整性。因此如何实现较低温度下在SiC纤维表面制备石墨界面，对提高SiCf/SiC复合材料的抗辐照性能、热导性能及力学性能至关重要。
发明内容
本发明的目的是为了解决现有制备SiCf/SiC复合材料采用的PyC界面在高剂量中子辐照后，界面发生退化，界面处产生裂缝，导致材料力学性能和导热性能降低等问题，提供一种低温SiC纤维表面石墨界面的制备方法；该方法首先在SiC纤维预制体表面沉积PyC界面，然后通过磁场及加热实现PyC界面的石墨化，在维持SiC纤维原有力学性能的同时提高SiCf/SiC复合材料的高温抗中子辐照能力。
本发明的目的是通过下述技术方案实现的。
一种低温条件下在SiC纤维表面制备石墨界面的方法，具体步骤如下：
步骤1、PyC界面的制备：采用化学气相沉积法在SiC纤维预制体中引入界面层，制备出SiC纤维预制体；所述界面层为热解碳PyC层；
步骤2、SiC纤维预制体的清洗：对SiC纤维预制体进行超声清洗并烘干；
步骤3、石墨界面的制备：采用强磁场辅助加热的方式使PyC界面石墨化；
步骤4、SiC纤维预制体的清洗：对SiC纤维预制体进行超声清洗并烘干，得到石墨界面。
所述步骤3中磁场强度为5～10特斯拉，磁场方向为沿纤维径向方向，加热温度为1000℃～1300℃，时间为30min～90min。
所述SiC纤维直径为12～14μm。
所述PyC界面的厚度为60～250nm。
所述石墨界面层的厚度为50～200nm。
有益效果
1、本发明的一种低温条件下在SiC纤维表面制备石墨界面的方法，在SiC纤维预制体表面引入一层PyC界面，通过调节磁场强度降低PyC界面的石墨化温度，从而获得厚度为50～200nm的石墨界面，提高SiCf/SiC复合材料的抗中子辐照能力。
2、同时，利用磁场辅助加热使PyC界面石墨化，可避免高温加热对SiC纤维的损伤，防止SiC纤维晶粒长大，保持SiC纤维力学强度，也会保证SiCf/SiC复合材料的力学性能。
附图说明
图1为采用该方法所制备的石墨界面的扫描电镜照片；
图2为采用该方法所制备的石墨界面处的EDS点扫描图；
图3为石墨层EDS元素成分分析；
图4为SiC纤维的EDS点扫描图；
图5为SiC纤维EDS元素成分分析；
图6为采用该方法所制备的含有石墨界面SiC纤维预制体的XRD图；
图7为采用该方法所制备的含有石墨界面SiC纤维预制体的TEM衍射图。
具体实施方式
现结合实施例与附图对本发明作进一步说明。
实施例1：
一种低温条件下在SiC纤维表面制备石墨界面的方法，石墨层厚度为50～200nm。采用化学气相沉积法在SiC纤维表面引入PyC界面，通过磁场下加热方式使PyC界面完全石墨化。
一种低温条件下在SiC纤维表面制备石墨界面的方法，具体步骤如下：
1、采用学气相沉积法，在SiC纤维预制体中引入一层PyC界面，沉积温度为900℃，厚度约为150nm，SiC纤维为厦门大学Amosic-3碳化硅纤维；
2、将SiC纤维预制体表面清洗干净，烘干；
3、将刷完表面带有PyC界面的SiC纤维预制体直接放入磁场加热设备中，氩气气氛保护下，调节磁场强度为6.0特斯拉，温度为1000℃，时间为30min，原位将PyC石墨化，得到石墨界面为120μm；
4、将SiC纤维预制体再次进行超声清洗并烘干，得到力学性能良好且完全包覆石墨界面的SiC纤维预制体；
5、对石墨界面进行SEM和EDS表征，图1-5表明石墨层均匀包覆SiC纤维表面；
6、对包覆石墨层SiC纤维进行XRD表征，无非晶石墨峰出现，且可观察到明显的石墨及SiC特征峰(图6)，PyC层在原位经过磁场加热后可完全石墨化；
7、对包覆120μm石墨界面的SiC纤维进行单丝拉伸强度测量，纤维单丝拉伸强度为2.98GPa，对比原始SiC纤维，其单丝拉伸强度未下降；
8、对包覆120μm石墨界面的SiC纤维进行TEM表征(图7)，对比原始SiC纤维，其平均晶粒尺寸未发生明显改变。
实施例2
一种低温SiC纤维表面石墨界面的制备方法，石墨层厚度为50～200nm。采用化学气相沉积法在SiC纤维表面引入PyC界面，通过磁场下加热方式使PyC界面完全石墨化。
一种低温SiC纤维表面石墨界面的制备方法，具体实施方法：
1、采用学气相沉积法，在SiC纤维预制体中引入一层PyC界面，沉积度为850℃，厚度约为60nm，SiC纤维为厦门大学Amosic-3碳化硅纤维；
2、将SiC纤维预制体表面清洗干净，烘干；
3、将刷完表面带有PyC界面的SiC纤维预制体直接放入磁场加热设备中，氩气气氛保护下，调节磁场强度为5.0特斯拉，温度为1100℃，时间为40min，原位将PyC石墨化，得到石墨界面为50μm；
4、将SiC纤维预制体再次进行超声清洗并烘干，得到力学性能良好且完全包覆石墨界面的SiC纤维预制体；
5、对石墨界面进行SEM和EDS表征，图片显示石墨层均匀包覆SiC纤维表面；
6、对包覆石墨层SiC纤维进行XRD表征，无非晶石墨峰出现，且可观察到明显的石墨及SiC特征峰，PyC层在原位经过磁场加热后可完全石墨化；
7、对包覆50μm石墨界面的SiC纤维进行单丝拉伸强度测量，纤维单丝拉伸强度为3.02GPa，对比原始SiC纤维，其单丝拉伸强度未下降；
8、对包覆50μm石墨界面的SiC纤维进行TEM表征，对比原始SiC纤维，其平均晶粒尺寸未发生明显改变。
实施例3
一种低温SiC纤维表面石墨界面的制备方法，石墨层厚度为50～200nm。采用化学气相沉积法在SiC纤维表面引入PyC界面，通过磁场下加热方式使PyC界面完全石墨化。
一种低温SiC纤维表面石墨界面的制备方法，具体实施方法：
1、采用学气相沉积法，在SiC纤维预制体中引入一层PyC界面，沉积度为950℃，厚度约为250nm，SiC纤维为厦门大学Amosic-3碳化硅纤维；
2、将SiC纤维预制体表面清洗干净，烘干；
3、将刷完表面带有PyC界面的SiC纤维预制体直接放入磁场加热设备中，氩气气氛保护下，调节磁场强度为8.0特斯拉，温度为1300℃，时间为70min，原位将PyC石墨化，得到石墨界面为200μm；
4、将SiC纤维预制体再次进行超声清洗并烘干，得到力学性能良好且完全包覆石墨界面的SiC纤维预制体；
5、对石墨界面进行SEM和EDS表征，图片显示石墨层均匀包覆SiC纤维表面；
6、对包覆石墨层SiC纤维进行XRD表征，无非晶石墨峰出现，且可观察到明显的石墨及SiC特征峰，PyC层在原位经过磁场加热后可完全石墨化；
7、对包覆200μm石墨界面的SiC纤维进行单丝拉伸强度测量，纤维单丝拉伸强度为2.94GPa，对比原始SiC纤维，其单丝拉伸强度未下降；
8、对包覆200μm石墨界面的SiC纤维进行TEM表征，对比原始SiC纤维，其平均晶粒尺寸未发生明显改变。
以上所述的具体描述，对发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施例而已，并不用于限定本发明的保护范围，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种低温条件下在SiC纤维表面制备石墨界面层的方法，其特征在于：具体步骤如下：
采用化学气相沉积法在SiC纤维预制体中引入界面层，制备出SiC纤维预制体；所述界面层为热解碳PyC层；
超声清洗并烘干；
采用磁场辅助加热的方式使PyC界面层石墨化，所述磁场强度为5~10特斯拉，磁场方向为沿纤维径向方向，加热温度为1000℃~1300℃，时间为30min~90min。
2.如权利要求1所述的一种低温条件下在SiC纤维表面制备石墨界面层的方法，其特征在于：所述PyC界面层的厚度为60~250nm。
3.如权利要求1所述的一种低温条件下在SiC纤维表面制备石墨界面层的方法，其特征在于：石墨界面层的厚度为50~200nm。
4.如权利要求1所述的一种低温条件下在SiC纤维表面制备石墨界面层的方法，其特征在于：使PyC界面层石墨化时处于惰性气体保护下进行。
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