CN110436955B - 一种钇改性SiCf/SiC陶瓷基复合材料及其制备方法 - Google Patents

一种钇改性SiCf/SiC陶瓷基复合材料及其制备方法 Download PDF

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CN110436955B
CN110436955B CN201910663654.5A CN201910663654A CN110436955B CN 110436955 B CN110436955 B CN 110436955B CN 201910663654 A CN201910663654 A CN 201910663654A CN 110436955 B CN110436955 B CN 110436955B
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刘虎
吕晓旭
齐哲
周怡然
杨金华
焦健
高晔
姜卓钰
艾莹珺
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AECC Beijing Institute of Aeronautical Materials
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Abstract

本发明涉及一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：制备含钇浆料、含钇碳化硅纤维预浸料、含钇成型体、含钇多孔碳预制体，通过熔融渗硅反应得到钇改性SiCf/SiC陶瓷基复合材料。本发明有效降低了复合材料基体中的游离硅含量，提高了复合材料的热导率和力学性能，同时具有良好的抗热震性能。

Description

一种钇改性SiCf/SiC陶瓷基复合材料及其制备方法
技术领域
本发明涉及一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，属于航空发动机用陶瓷基复合材料制备领域。
背景技术
连续碳化硅纤维增强碳化硅(SiCf/SiC)陶瓷基复合材料具有耐高温、密度低、热稳定性好等优点，将其应用于航空发动机可提高涡轮前进口温度、减轻结构重量、减少冷气用量、提高燃烧效率。国外已有报道将该材料应用于航空发动机燃烧室、涡轮等热端部件，实现了发动机性能的大幅提升。
经过数十年的研究，现已发展出多种SiCf/SiC陶瓷基复合材料制备工艺，其中熔渗工艺是在高温下将液态熔融硅引入多孔碳基体中，快速反应生成致密的碳化硅基体，具有制造周期短、生产成本低、可实现近净成型等优势，成为极具工程化前景的陶瓷基复合材料制备工艺之一。但目前熔渗工艺制备的 SiCf/SiC陶瓷基复合材料不可避免地在基体中残余一定量的硅，导致复合材料高温下的蠕变性能较差；此外，当复合材料的使用温度超过硅的熔点时(>1412℃)，硅的熔化使得复合材料力学性能急剧下降。
因此，降低SiCf/SiC陶瓷基复合材料基体中的硅含量对该材料在高温下的可靠使用尤为重要。已有文献报道研究人员采用Si-Mo、Si-Ti或Si-Zr等合金代替纯Si作为熔渗剂，使游离硅转化成为相应的硅化物，可在一定程度上降低了基体中的游离硅含量(Development of a high temperature Cf/XSi2–SiC(X＝Mo,Ti) composite viareactive melt infiltration；Effect of infiltration time on the microstructureand mechanical properties of C/C-SiC composite prepared by Si-Zr10 alloyedmelt infiltration等)；专利CN 107540411 A中采用Ti粉对残余硅进行后处理，反应生成TiSi2后使游离硅的含量下降。但新生成的硅化物热膨胀系数比碳化硅基体大得多，如MoSi2、TiSi2分别为9×10-6/K、10.4×10-6/K，而SiC仅约为4.5×10-6/K，由于热膨胀系数相差过大，导致在升温-降温的反复循环中，复合材料极易因热不匹配而出现裂纹等缺陷。
发明内容
本发明的目的是：本发明即是针对现有技术的不足，提供一种钇改性 SiCf/SiC陶瓷基复合材料的制备方法，不仅有效降低了基体中的游离硅含量，还避免出现热膨胀系数失配等问题，同时复合材料还具有较高的热导率和优异的力学性能。
本发明的技术方案是：
提供一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
步骤1、制备含钇料浆
将钇粉、粘结剂、造孔剂、助剂和溶剂混合后，再加入研磨球，球磨12～24 小时后得到含钇料浆；
步骤2、制备含钇碳化硅纤维预浸料
将含钇料浆涂覆在碳化硅纤维织物表面，然后在20～25℃下晾置1～12小时，得到纤维预浸料；
步骤3、制备含钇成型体
铺叠6～20层所述的纤维预浸料，经热压成型后得到含钇成型体；
步骤4、制备含钇多孔碳预制体
将含钇成型体置于加热炉中进行碳化，加热温度为800～1000℃，碳化时间为0.5～6小时，碳化的气氛为氩气，碳化后得到含钇多孔碳预制体；
步骤5、制备钇改性SiCf/SiC陶瓷基复合材料
在石墨坩埚的内表面涂覆氮化硼，将硅粉和所述含钇多孔碳预制体置于石墨坩埚内，将石墨坩埚置于真空加热环境，加热温度为1420～1600℃，加热时间为0.5～4小时，真空度为0.1～100Pa，得到钇改性SiCf/SiC陶瓷基复合材料。
进一步的，所述含钇料浆中各组分的质量份数为：钇粉15～30份，粘结剂 20～50份，造孔剂5～10份，助剂2～5份，溶剂50～100份。
进一步的，所述碳化硅纤维织物表面沉积了0.1～2μm的氮化硼界面层和 0.1～2μm的碳化硅界面层。
进一步的，所述钇粉的粒径为0.5～10μm。
进一步的，所述粘结剂为酚醛树脂、苯并噁嗪树脂、环氧树脂中任意两种的混合物。
进一步的，所述造孔剂为纤维素、聚乙二醇、聚甲基丙烯酸甲酯微球、聚苯乙烯微球中的一种或两种的组合。
进一步的，所述助剂包括基材润湿剂、消泡剂、防沉剂。
进一步的，所述溶剂为乙醇、异丙醇、乙酸甲酯、乙酸丁酯、丙酮、乙二醇单乙醚、乙二醇单丁醚、丙二醇单甲醚和丙二醇单丁醚中的两种或多种的组合。
其中，所述含钇多孔碳预制体的孔隙率为45％～65％；所述钇改性SiCf/SiC 陶瓷基复合材料的热导率大于30W/m·K、拉伸强度大于350MPa。
本发明的优点是：与现有技术相比，本发明钇改性SiCf/SiC陶瓷基复合材料的制备方法具有以下优点：①本方法将SiCf/SiC复合材料中残余硅的质量分数降低至0.03％以内，提高了复合材料的高温蠕变性能、耐水氧性能以及耐燃气热腐蚀性能；②钇与硅原位生成钇的硅化物后，填充了基体中的孔隙，使复合材料具有较高的热导率，可满足航空发动机热端部件高温下的热量传导要求；同时，所生成的钇的硅化物具有较高的熔点，提高了复合材料的使用温度；③所制备的SiCf/SiC复合材料基体无热不匹配等问题，从而具有优良的抗热震性能，经1000次热震试验(1200℃
Figure GDA0003140746820000041
室温循环1000次)后，基体无裂纹出现；④本方法在复合材料基体生成过程中即实现了残余硅含量的控制，无需再经后处理，工艺简便，可操作性强。
具体实施方式
下面结合实施例对本发明做进一步详细说明。
实施例1
本实施例提供的钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
(1)制备含钇料浆：将17份粒径为3.5μm的钇粉、25份粘结剂(由20 份酚醛树脂和5份苯并噁嗪树脂组成)、5份造孔剂(由5份纤维素组成)、3份助剂(由1份基体润湿剂、1份消泡剂、1份防沉剂组成)、60份溶剂(由30份乙醇和30份乙酸丁酯组成)混合后，加入研磨珠，球磨12h得到含钇料浆；
(2)制备含钇碳化硅纤维预浸料：将含钇料浆涂覆在表面沉积了0.25μm 氮化硼界面层和1.86μm碳化硅界面层的碳化硅纤维布表面，然后在23℃下晾置4h；
(3)制备含钇成型体：将10层含钇碳化硅纤维预浸料铺叠在一起，经热压成型后得到含钇成型体；
(4)制备含钇多孔碳预制体：将含钇成型体转入加热炉中，在900℃氩气氛下碳化处理2h得到孔隙率为52％的含钇多孔碳预制体；
(5)制备钇改性SiCf/SiC陶瓷基复合材料：将硅粉铺覆于内表面涂覆氮化硼涂层的石墨坩埚内，然后将含钇多孔碳预制体置于硅粉表面，在1500℃真空条件下反应2小时得到钇改性SiCf/SiC陶瓷基复合材料。
经测试，所制备的钇改性SiCf/SiC陶瓷基复合材料的热导率为32.3W/m·K、拉伸强度为387MPa；经1000次热震试验(1200℃
Figure GDA0003140746820000051
室温循环1000次)后，基体无裂纹出现。
实施例2
本实施例提供的钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
(1)制备含钇料浆：将28份粒径为8.5μm的钇粉、50份粘结剂(由45 份酚醛树脂和5份环氧树脂组成)、10份造孔剂(由4份聚乙二醇和6份聚苯乙烯微球组成)、5份助剂(由3份基体润湿剂、1份消泡剂、1份防沉剂组成)、 100份溶剂(由10份乙醇、12份丙二醇单甲醚、3份丙酮、75份乙酸甲酯组成) 混合后，加入研磨珠，球磨24h得到含钇料浆；
(2)制备含钇碳化硅纤维预浸料：将含钇料浆涂覆在表面沉积了0.85μm 氮化硼界面层和0.5μm碳化硅界面层的碳化硅纤维布表面，然后在23℃下晾置 10h；
(3)制备含钇成型体：将18层含钇碳化硅纤维预浸料铺叠在一起，经热压成型后得到含钇成型体；
(4)制备含钇多孔碳预制体：将含钇成型体转入加热炉中，在1000℃氩气氛下碳化处理6h得到孔隙率为63％的含钇多孔碳预制体；
(5)制备钇改性SiCf/SiC陶瓷基复合材料：将硅粉铺覆于内表面涂覆氮化硼涂层的石墨坩埚内，然后将含钇多孔碳预制体置于硅粉表面，在1580℃真空条件下反应4小时得到钇改性SiCf/SiC陶瓷基复合材料。
经测试，所制备的钇改性SiCf/SiC陶瓷基复合材料的热导率为31.5W/m·K、拉伸强度为369MPa；经1000次热震试验(1200℃
Figure GDA0003140746820000061
室温循环1000次)后，基体无裂纹出现。
实施例3
本实施例提供的钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
(1)制备含钇料浆：将18份粒径为5.5μm的钇粉、42份粘结剂(由36 份苯并噁嗪树脂和6份酚醛树脂组成)、9份造孔剂(由3份聚乙二醇和6份聚甲基丙烯酸甲酯微球组成)、5份助剂(由2份基体润湿剂、2份消泡剂、1份防沉剂组成)、85份溶剂(由5份乙醇、20份丙二醇单甲醚、60份醋酸丁酯组成) 混合后，加入研磨珠，球磨18h得到含钇料浆；
(2)制备含钇碳化硅纤维预浸料：将含钇料浆涂覆在表面沉积了1.64μm 氮化硼界面层和0.28μm碳化硅界面层的碳化硅纤维布表面，然后在25℃下晾置3h；
(3)制备含钇成型体：将12层含钇碳化硅纤维预浸料铺叠在一起，经热压成型后得到含钇成型体；
(4)制备含钇多孔碳预制体：将含钇成型体转入加热炉中，在850℃氩气氛下碳化处理4h得到孔隙率为48％的含钇多孔碳预制体；
(5)制备钇改性SiCf/SiC陶瓷基复合材料：将硅粉铺覆于内表面涂覆氮化硼涂层的石墨坩埚内，然后将含钇多孔碳预制体置于硅粉表面，在1425℃真空条件下反应3.5小时得到钇改性SiCf/SiC陶瓷基复合材料。
经测试，所制备的钇改性SiCf/SiC陶瓷基复合材料的热导率为34.2W/m·K、拉伸强度为403MPa；经1000次热震试验(1200℃
Figure GDA0003140746820000071
室温循环1000次)后，基体无裂纹出现。
实施例4
本实施例提供的钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
(1)制备含钇料浆：将21份粒径为0.8μm的钇粉、36份粘结剂(由18 份苯并噁嗪树脂和18份环氧树脂组成)、6份造孔剂(由6份聚甲基丙烯酸甲酯微球组成)、4份助剂(由2份基体润湿剂、1份消泡剂、1份防沉剂组成)、65 份溶剂(由5份异丙醇、20份乙二醇单乙醚、40份醋酸丁酯组成)混合后，加入研磨珠，球磨15h得到含钇料浆；
(2)制备含钇碳化硅纤维预浸料：将含钇料浆涂覆在表面沉积了1.25μm 氮化硼界面层和1.52μm碳化硅界面层的碳化硅纤维布表面，然后在25℃下晾置9h；
(3)制备含钇成型体：将6层含钇碳化硅纤维预浸料铺叠在一起，经热压成型后得到含钇成型体；
(4)制备含钇多孔碳预制体：将含钇成型体转入加热炉中，在850℃氩气氛下碳化处理1h得到孔隙率为56％的含钇多孔碳预制体；
(5)制备钇改性SiCf/SiC陶瓷基复合材料：将硅粉铺覆于内表面涂覆氮化硼涂层的石墨坩埚内，然后将含钇多孔碳预制体置于硅粉表面，在1490℃真空条件下反应1小时得到钇改性SiCf/SiC陶瓷基复合材料。
经测试，所制备的钇改性SiCf/SiC陶瓷基复合材料的热导率为31.9W/m·K、拉伸强度为353MPa；经1000次热震试验(1200℃
Figure GDA0003140746820000081
室温循环1000次)后，基体无裂纹出现。

Claims (8)

1.一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，包括以下步骤：
步骤1、制备含钇料浆
将钇粉、粘结剂、造孔剂、助剂和溶剂混合后，再加入研磨球，球磨12～24小时后得到含钇料浆；
步骤2、制备含钇碳化硅纤维预浸料
将含钇料浆涂覆在碳化硅纤维织物表面，然后在20～25℃下晾置1～12小时，得到纤维预浸料；
步骤3、制备含钇成型体
铺叠6～20层所述的纤维预浸料，经热压成型后得到含钇成型体；
步骤4、制备含钇多孔碳预制体
将含钇成型体置于加热炉中进行碳化，加热温度为800～1000℃，碳化时间为0.5～6小时，碳化的气氛为氩气，碳化后得到含钇多孔碳预制体；
步骤5、制备钇改性SiCf/SiC陶瓷基复合材料
在石墨坩埚的内表面涂覆氮化硼，将硅粉和所述含钇多孔碳预制体置于石墨坩埚内，将石墨坩埚置于真空加热环境，加热温度为1420～1600℃，加热时间为0.5～4小时，真空度为0.1～100Pa，得到钇改性SiCf/SiC陶瓷基复合材料。
2.如权利要求1所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述含钇料浆中各组分的质量份数为：钇粉15～30份，粘结剂20～50份，造孔剂5～10份，助剂2～5份，溶剂50～100份。
3.如权利要求1所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述碳化硅纤维织物表面沉积了0.1～2μm的氮化硼界面层和0.1～2μm的碳化硅界面层。
4.如权利要求1所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述钇粉的粒径为0.5～10μm。
5.如权利要求2所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述粘结剂为酚醛树脂、苯并噁嗪树脂、环氧树脂中任意两种的混合物。
6.如权利要求2所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述造孔剂为纤维素、聚乙二醇、聚甲基丙烯酸甲酯微球、聚苯乙烯微球中的一种或两种的组合。
7.如权利要求2所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述助剂包括基材润湿剂、消泡剂、防沉剂。
8.如权利要求2所述的一种钇改性SiCf/SiC陶瓷基复合材料的制备方法，其特征在于：所述溶剂为乙醇、异丙醇、乙酸甲酯、乙酸丁酯、丙酮、乙二醇单乙醚、乙二醇单丁醚、丙二醇单甲醚和丙二醇单丁醚中的两种或多种的组合。
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