CN110330353A - 一种SiCf/SiC复合材料火焰筒及其自动化制备方法 - Google Patents

一种SiCf/SiC复合材料火焰筒及其自动化制备方法 Download PDF

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CN110330353A
CN110330353A CN201910688219.8A CN201910688219A CN110330353A CN 110330353 A CN110330353 A CN 110330353A CN 201910688219 A CN201910688219 A CN 201910688219A CN 110330353 A CN110330353 A CN 110330353A
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sic
inner liner
burner inner
layer
composite material
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CN110330353B (zh
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阳海棠
郭小军
黄小忠
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Central South University
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Central South University
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Priority to PCT/CN2020/101903 priority patent/WO2021027469A1/zh
Priority to US17/474,091 priority patent/US11591267B2/en
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Abstract

一种SiCf/SiC复合材料火焰筒的自动化制备方法，包括如下步骤：将SiC纤维采用化学气相沉积法制备界面层，得到带连续界面层的SiC纤维；根据仿真模拟计算得到的纤维体积和纤维走向，将得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，获得净尺寸成型的预制体；对得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理；然后在得到的预制体表面制备环境障碍涂层；最后继续在表面制备热障涂层，全智能化得到高致密度SiCf/SiC复合材料火焰筒；本发明制备得到的SiCf/SiC复合材料火焰筒不仅具有耐高温、长寿命的特点，还具有低热膨胀系数、高热导率和高抗热震性能以及力学性能优异等优势，同时制备方法自动化程度高、生产周期短、成本低且质量可控。

Description

一种SiCf/SiC复合材料火焰筒及其自动化制备方法
技术领域
本发明涉及航空用结构材料技术领域，具体涉及一种SiCf/SiC复合材料火焰筒及其自动化制备方法。
背景技术
燃烧室是航空发动机的核心部件之一，其主要功能是将燃料的化学能经过燃烧转变为热能，以提高燃气在涡轮和喷管中膨胀的能力，在燃烧室的结构组成中，火焰筒是组织燃烧的场所，是保证空气分股、燃烧充分、掺混均匀并使壁面得到有效冷却的关键部件，燃烧室的可靠性、经济性和寿命在很大程度上取决于火焰筒的可靠性和耐温程度，因此研制高性能长寿命的燃烧室火焰筒对于提高发动机性能起着至关重要的作用。
现有的碳化硅纤维增强陶瓷基(SiCf/SiC)复合材料具有优异的性能，是代替高温合金作为航空发动机热端构件用材料的首选材料，然而服役环境中的应力作用会促使复合材料基体开裂，加速材料的损伤和腐蚀，影响其在高温燃气环境下服役长寿命的要求，从而严重制约SiCf/SiC复合材料在发动机燃烧室火焰筒的应用；如US20120076927A1的专利，提供了一种改善纤维增强硅碳复合材料的机械性能的方法，专利中通过对复合材料进行控制热处理，改进了纤维界面涂层和陶瓷基体，同时可以除去相基质中多余的硅，但是该专利中对处理时间-温度-环境条件的限定十分苛刻，热处理甚至达到1900℃的处理温度，在真空中或在纯度大于99％的惰性气体环境中处理保持时间长达100小时，另外单纯采用CVI工艺制备陶瓷基，虽然能有效控制游离硅，但是不能保证材料的高致密性，不利于应用于市场，所以研发一种可低成本制备高致密度，同时还能除去多余硅的高性能SiCf/SiC复合材料火焰筒的制备方法显得尤为必要；
另外专利CN106966738B中采用三维四步法编织燃烧室火焰筒预制体，而连接部分采用纤维缝合技术，当火焰筒处于高温燃气环境中，会在连接处形成应力集中和轻微开裂，从而加速材料的损伤和腐蚀，严重制约着复合材料火焰筒性能的发挥；而且通过图1所示有限元法分析火焰筒温度场分布图可以看出，火焰筒冷、热端之间具有约240℃的温差，并且火焰筒内部的温度变化梯度较大，所以温差会使材料内部产生应力，进而产生裂纹，所以要求火焰筒必须具有低的热膨胀系数，以保证温度变化时构件尺寸的稳定性，同时，必须具有高热导率，避免因为热应力集中而造成的火焰筒失效；同时目前三维四步的编织方法基本全部采用手工编织的方式，成本高、工期长、质量不可控，因此研制自动化的连续制备火焰筒预制体对于SiCf/SiC复合材料在火焰筒的广泛应用有至关重要的作用。
发明内容
针对现有技术存在的上述问题，本申请提供了一种SiCf/SiC复合材料火焰筒及其自动化制备方法，制备得到的SiCf/SiC复合材料火焰筒不仅具有耐高温、长寿命的特点，还具有低热膨胀系数、高热导率和高抗热震性能以及力学性能优异等优势，同时制备方法自动化程度高、生产周期短、成本低且质量可控。
本发明的技术方案如下：一种SiCf/SiC复合材料火焰筒的自动化制备方法，包括如下步骤：
1)将SiC纤维采用化学气相沉积法制备界面层，得到带连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，获得净尺寸成型的预制体；
3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1～1∶2；
4)在步骤3)得到的预制体表面制备环境障碍涂层，所述环境障碍涂层的厚度为60～150um；
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层的厚度为100～150um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
本发明仿真模拟包括有限元分析法分析温度场、以及联合采用多尺度分析与有限元实体建模相结合的方法，根据温度场分析、指导复合材料火焰筒构件的设计、纤维体积、纤维走向以及复合材料的成型方式等参数，以达到提高SiCf/SiC复合材料火焰筒性能预测的效率和精度，实现制备方法的自动化和高效性的目的。
本发明所述步骤1)中的界面层为PyC、SiC、B4C、ZrC、HfC、TaC、Si3N4、BN中的一种或多种。
本发明所述化学气相沉淀工艺具体为：根据引入的界面层选择前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500～1400℃，沉积压力为0.5～12KPa，沉积时间为60～600min，沉积的界面层厚度为100nm～2μm；所述前驱体为甲烷、三氯甲基硅烷、氯化硼、氯化锆、氯化钽、氯化硅、卤化硼、氨气中的一种或几种。
本发明所述步骤2)单向带铺带、缠绕成型包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2～3次的环氧树脂脱模剂，并对火焰筒模具加热到30～50℃；
步骤二、将体积含量为40～65％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为50～70％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，由内向外以缠绕张力梯度递减的方式进行缠绕，缠绕角度为30～90°，缠绕速度为0.3～0.7m/s，缠绕张力为2～10N/cm，缠绕厚度为1～5mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为90～165℃，固化时间为4～8h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用磨削加工及激光加工相结合方式进行产品精加工，即得到净尺寸成型的预制件。
本发明所述步骤3)反应熔体浸渗工艺具体为熔融渗硅工艺：设备为真空高温气氛沉积炉和真空高温渗硅炉，以硅合金为硅源，氩气为稀释气体，沉积温度为1450～1800℃，沉积压力为2Pa～常压，渗硅时间为30～300min；所述硅合金为Si与Ta、Hf、Mo、W、Zr、Ti、B、Be的二元或三元的合金。
本发明所述步骤3)的化学气相沉积工艺具体为，以三氯甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度900～1200℃，沉积压力为0.5～5KPa，沉积时间为60～6000min。
本发明所述步骤4)中的环境障碍涂层包括Si粘结层、稀土单硅酸盐Re2SiO5面层、以及位于所述粘结层和面层之间的Yb2Si2O7中间层；所述Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1～2：1～2：1～3；所述稀土单硅酸盐Re2SiO5选自Y2SiO5、Sc2SiO5、Gd2SiO5、Er2SiO5、Tm2SiO5、Yb2SiO5、Lu2SiO5中的至少一种。
本发明所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Re2SiO5分别进行球磨处理，直至粒径为20～80um；
(2)将预制件置于惰性保护气氛中，在1450～1800℃下热处理1～4h，形成Si粘结层；
(3)采用等离子体喷涂法，将Yb2Si2O7粉体喷涂在带有Si粘结层的预制件上，形成中间层；
(4)采用等离子体喷涂法，将稀土单硅酸盐Re2SiO5粉体喷涂在带有粘结层和中间层的预制件上，得到所述环境障碍涂层。
所述等离子喷涂法的参数包括：等离子气体包括氩气与氦气，所述氩气的流量为60～80slpm，所述氦气的流量为40～60slpm，送粉速率为10～35r/min，喷涂距离为90～200mm。
本发明所述步骤5)所述热障涂层为R2O3、ZrO2、CeO2、Al2O3·2SiO2、SrZrO3、La2Zr2O7、La2Ce2O7中的至少一种。
本发明还提供了一种SiCf/SiC复合材料火焰筒。
本发明有益的技术效果在于：
(1)本发明在纤维与基体之间引入均匀界面层，使得纤维与基体不会融为一体，层次分明的纤维-界面层-基体结构能够吸收裂纹扩散所需要的能量，有效提高了复合材料的力学强度；同时陶瓷界面层的存在，能够保护SiC纤维遭受氧气、水蒸气、燃油、酸等的腐蚀，从而提高使用温度与使用环境。
(2)本发明联合采用化学气相沉积工艺(CVI)和反应熔渗工艺(MI)对陶瓷基复合材料进行致密化处理，一方面MI工艺简单，周期短，MI-SiC/SiC具有更高的密度和更低的显气孔率，因此复合材料具有更高的热导率，尤其是垂直纤维方向的热导率，MI-SiC/SiC是CVI-SiC/SiC复合材料的2倍多，有利于抗热震性能的改善，另一方面根据实验数据得知MI-SiC/SiC复合材料的热膨胀系数大于CVI-SiC/SiC复合材料，而通过优化工艺参数，调控复合材料基体组成与结构，从而实现材料热膨胀系数的可调控性，并获得具有低热膨胀系数的材料和空间光学用支撑构件，有效降低材料受热不均产生的形变程度，提高SiCf/SiC复合材料火焰筒的使用寿命；同时本发明采用反应熔渗工艺中的处理温度低于常规温度，可有效降低复合材料表面的硅含量，从而提高复合材料的耐高温性能。
(3)本发明根据仿真模拟计算得到的纤维体积和纤维走向，采用单向带铺带、缠绕成型的自动化方式进行预制件的制备，使得在获得三维预制体的同时，延厚度方向，纤维布间的距离达到最低，且纤维布都保持平整性，这样既提高了纤维体积含量，还保证了纤维的分布均匀性，该方法制成的复合材料火焰筒具有轻质、强度高、无微裂纹的优势，同时还具有耐高温、抗磨损、防渗漏的特点，同时自动化程度高、生产周期短、成本低且质量可控。
(4)本发明中的环境障碍涂层选用Si层，考虑Si具有更高的熔点，因此可以保证环境障碍涂层具有更高的环境适用温度；中间层材料采用Yb2Si2O7，考虑Yb2Si2O7的热膨胀系数较小，显著低于稀土单硅酸盐Re2SiO5面层的热膨胀系数，使得在热循环过程中，不容易被裂纹贯穿，有利于提高涂层的抗热震性能，另一方面本发明稀土硅酸盐Re2SiO5面层具有优异的耐水蒸气腐蚀性能，可以进一步提高涂层体系的防护性能。
(5)本发明在制备Si层中，采用高温反应热处理的方法形成Si层，可以进一步降低复合材料表面的硅含量，从而提高复合材料的耐高温性能，另一方面通过优化热处理温度提高碳化硅涂层的晶粒尺寸和涂层致密度，从而获得耐高温、致密度高的复合材料火焰筒。
(6)本发明首先通过有限元法分析复合材料火焰筒的温度场，然后采用多尺度分析与有限元实体建模相结合的方法，将细观、宏观相结合，获取结构的确定性载荷以及载荷处的纤维基体状态，进行指导复合材料火焰筒构件的设计、纤维体积、纤维走向以及复合材料的成型方式等参数，提高了SiCf/SiC复合材料火焰筒性能预测的效率和精度，实现制备方法的自动化和高效性。
附图说明
图1为本发明SiCf/SiC复合材料火焰筒有限元计算的温度场示意图。
图2为本发明SiCf/SiC复合材料火焰筒的制备流程示意图。
图3为实施例3的PyC/Si3N4/BN多层界面层的扫描电镜图。
图4为本发明MI SiC/CVI SiC基体的扫描电镜图。
图5为本发明EBC环境障碍层的扫描电镜图。
图6为本发明EBC环境障碍层的表面放大图。
图7为本发明的热防护涂层结构设计图。
图8为本发明单向带铺放、缠绕成型的结构示意图。
图9为本发明SiCf/SiC复合材料火焰筒的立体图。
图10为实施例1经1100℃×20min热震不同次数后的表观状态和截面形貌。
图11为实施例1经1200℃×20min热震不同次数后的表观状态和截面形貌。
图12为实施例1经1300℃×20min热震不同次数后的表观状态和截面形貌。
下面结合附图和实施例，对本发明进行具体描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例，基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
以下结合具体优选实施例对本发明一种SiCf/SiC复合材料火焰筒的制备方法进行详细阐述。
实施例1：
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中，以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500℃，沉积压力为12KPa，沉积时间为600min，沉积的界面层厚度为100nm；随炉冷却后，即得到带连续PyC界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂，并对火焰筒模具加热到30℃；
步骤二、将体积含量为40％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为50％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为30°，缠绕速度为0.3m/s，缠绕张力为2N/cm，缠绕厚度为1mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为90℃，固化时间为4h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件；
3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理，先进行低温真空渗硅，以Si与Ta的二元合金作为硅源，氩气为稀释气体，沉积温度为1400℃，沉积压力为常压，渗硅时间为300min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为900℃，沉积压力为5KPa，沉积时间为6000min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：1；
4)在步骤3)得到的预制体表面制备60um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为20um；
(2)将预制件置于惰性保护气氛中，在1450℃下热处理4h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1：1：1，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为60slpm，所述氦气的流量为40slpm，送粉速率为10r/min，喷涂距离为90mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-Al2O3，厚度为100um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
实施例2：
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中，以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1400℃，沉积压力为0.5KPa，沉积时间为60min，沉积的界面层厚度为2um；随炉冷却后，即得到带连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆3次的环氧树脂脱模剂，并对火焰筒模具加热到50℃；
步骤二、将体积含量为65％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为70％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为90°，缠绕速度为0.7m/s，缠绕张力为10N/cm，缠绕厚度为5mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为165℃，固化时间为8h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理，先进行低温真空渗硅，以Si与Ta的二元合金作为硅源，氩气为稀释气体，沉积温度为1800℃，沉积压力为2Pa，渗硅时间为30min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1200℃，沉积压力为0.5KPa，沉积时间为60min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：2；
4)在步骤3)得到的预制体表面制备150um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为80um；
(2)将预制件置于惰性保护气氛中，在1800℃下热处理1h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为2：2：3，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为80slpm，所述氦气的流量为60slpm，送粉速率为35r/min，喷涂距离为200mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-Al2O3，厚度为150um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
实施例3
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维置于PyC界面层相应的化学气相沉积温度的电阻炉中，以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为8KPa，沉积时间为300min，沉积的界面层厚度为1um；随炉冷却后，即得到带连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂，并对火焰筒模具加热到40℃；
步骤二、将体积含量为55％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为60％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为60°，缠绕速度为0.5m/s，缠绕张力为6N/cm，缠绕厚度为3mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为120℃，固化时间为6h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理，先进行低温真空渗硅，以Si与Ta的二元合金作为硅源，氩气为稀释气体，沉积温度为1600℃，沉积压力为1Pa，渗硅时间为180min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为3KPa，沉积时间为4800min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：1.5；
4)在步骤3)得到的预制体表面制备100um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为50um；
(2)将预制件置于惰性保护气氛中，在1600℃下热处理3h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1：2：1，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为70slpm，所述氦气的流量为50slpm，送粉速率为20r/min，喷涂距离为120mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-Al2O3，厚度为120um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
实施例4
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维先后置于PyC界面层、Si3N4界面层和BN界面层相应的化学气相沉积温度的电阻炉中，引入PyC/Si3N4/BN多层界面层，具体的引入PyC界面层以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500℃，沉积压力为12KPa，沉积时间为600min，沉积的界面层厚度为100nm；具体的引入Si3N4界面层以三氯甲基硅烷和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500℃，沉积压力为0.5KPa，沉积时间为600min，沉积的界面层厚度为100nm；具体的引入BN界面层以氯化硼和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500℃，沉积压力为12KPa，沉积时间为600min，沉积的界面层厚度为100nm；随炉冷却后，即得到带多层连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂，并对火焰筒模具加热到30℃；
步骤二、将体积含量为40％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为50％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为30°，缠绕速度为0.3m/s，缠绕张力为2N/cm，缠绕厚度为1mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为90℃，固化时间为4h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理，先进行低温真空渗硅，以Si与Mo的二元合金作为硅源，氩气为稀释气体，沉积温度为1400℃，沉积压力为2Pa，渗硅时间为300min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为900℃，沉积压力为5KPa，沉积时间为60min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：1；
4)在步骤3)得到的预制体表面制备60um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为20um；
(2)将预制件置于惰性保护气氛中，在1450℃下热处理4h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1：1：1，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为60slpm，所述氦气的流量为40slpm，送粉速率为10r/min，喷涂距离为90mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-ZrO2-CeO2，厚度为100um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
实施例5
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维先后置于PyC界面层、Si3N4界面层和BN界面层相应的化学气相沉积温度的电阻炉中，引入PyC/Si3N4/BN多层界面层，具体的引入PyC界面层以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1400℃，沉积压力为0.5KPa，沉积时间为60min，沉积的界面层厚度为2um；具体的引入Si3N4界面层以三氯甲基硅烷和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1400℃，沉积压力为0.5KPa，沉积时间为60min，沉积的界面层厚度为2um；具体的引入BN界面层以氯化硼和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1400℃，沉积压力为0.5KPa，沉积时间为60min，沉积的界面层厚度为2um；随炉冷却后，即得到带多层连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂，并对火焰筒模具加热到50℃；
步骤二、将体积含量为65％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为70％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为90°，缠绕速度为0.7m/s，缠绕张力为10N/cm，缠绕厚度为5mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为90℃，固化时间为4h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理，先进行低温真空渗硅，以Si与Mo的二元合金作为硅源，氩气为稀释气体，沉积温度为1800℃，沉积压力为常压，渗硅时间为30min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1200℃，沉积压力为0.5KPa，沉积时间为6000min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：2；
4)在步骤3)得到的预制体表面制备150um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为80um；
(2)将预制件置于惰性保护气氛中，在1800℃下热处理1h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为2：2：3，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为80slpm，所述氦气的流量为60slpm，送粉速率为35r/min，喷涂距离为200mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-ZrO2-CeO2，厚度为150um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
实施例6
本实施例提供了一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维先后置于PyC界面层、Si3N4界面层和BN界面层相应的化学气相沉积温度的电阻炉中，引入PyC/Si3N4/BN多层界面层，具体的引入PyC界面层以甲烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为8KPa，沉积时间为300min，沉积的界面层厚度为1um；具体的引入Si3N4界面层以三氯甲基硅烷和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为8KPa，沉积时间为300min，沉积的界面层厚度为1um；具体的引入BN界面层以氯化硼和氨气为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为8KPa，沉积时间为300min，沉积的界面层厚度为1um；随炉冷却后，即得到带多层连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2次的环氧树脂脱模剂，并对火焰筒模具加热到40℃；
步骤二、将体积含量为55％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为60％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，缠绕角度为60°，缠绕速度为0.5m/s，缠绕张力为6N/cm，缠绕厚度为3mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为120℃，固化时间为6h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用激光加工方式进行产品精加工，即得到净尺寸成型的预制件。
3)对步骤2)得到的预制体先后采用化学气相沉积工艺和反应熔体浸渗工艺进行致密化处理，先进行低温真空渗硅，以Si与Mo的二元合金作为硅源，氩气为稀释气体，沉积温度为1600℃，沉积压力为1Pa，渗硅时间为180min，采用随炉冷却，重复1次；再进行化学气相沉积，以三甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为1000℃，沉积压力为3KPa，沉积时间为4800min，采用随炉冷却，重复1次，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1：1.5；
4)在步骤3)得到的预制体表面制备100um厚的环境障碍涂层，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Yb2Si2O5分别进行球磨处理，直至粒径为60um；
(2)将预制件置于惰性保护气氛中，在1600℃下热处理2h，形成Si粘结层；
(3)按照Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1：2：1，对中间层和面层进行制备，制备过程中均采用等离子体喷涂法，具体为等离子气体包括氩气与氦气，所述氩气的流量为70slpm，所述氦气的流量为50slpm，送粉速率为20r/min，喷涂距离为150mm，依次将Yb2Si2O7粉体和Yb2Si2O5粉体喷涂在预制件上，得到高致密度全智能化的SiCf/SiC复合材料火焰筒。
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层为R2O3-ZrO2-CeO2，厚度为120um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
测试例
将实施例一到实施例六制备得到的SiCf/SiC复合材料火焰筒进行性能测试，并且将常规的火焰筒作为对比例，具体如下：
1、高温耐氧化性能
测定方法：将实施例一到实施例六制备的SiCf/SiC复合材料火焰筒截取试样，制成尺寸为3×4×40(mm)的力学性能件，对试件进行500h的有氧环境、常温和高温环境处理，其中高温环境分别为1400℃和1600℃。
测试结果：测试的弯曲强度结果如下表1所示：
表1 不同温度下SiCf/SiC复合材料火焰筒的弯曲强度
2、密度和孔隙率
测定方法：将实施例一至六制备得到的SiCf/SiC复合材料火焰筒根据GB/T1966-1996《多孔陶瓷显气孔率、容量试验方法》进行检测。
测定结果：制备得到的SiCf/SiC复合材料火焰筒的体积密度为2.75g/m3，显孔隙率为0.65％。
3、抗热震性能
测定方法：将实施例一至六制备得到的SiCf/SiC复合材料火焰筒上切割试样件，分别放置在完全密闭的空间内，分别加热至1100℃、1200℃、1300℃，接着置于20℃水中，反复的升温、冷却处理，目测有无开裂现象。
测定结果：测试的抗震性能如下表2所示：
表2 不同温度下SiCf/SiC复合材料火焰筒的抗热震性能
抗热震性能的优劣通过升温、冷却处理的次数表示，次数越多，抗热震性能越好；从表2中可以看出实施例一至六的抗热震性能更加优异。
4、热导率
测定方法：将实施例一至六制备得到的SiCf/SiC复合材料火焰筒根据GB/T17911.8-2002《耐火陶瓷纤维制品导热系数试验方法》进行检测。
测定结果：制备得到的SiCf/SiC复合材料火焰筒的平均热导率为30W/(m·K)。
5、热膨胀系数
测定方法：将实施例一至六制备得到的SiCf/SiC复合材料火焰筒根据GB/T16535-1996《工程陶瓷线热膨胀系数试验方法》进行检测。
测定结果：制备得到的SiCf/SiC复合材料火焰筒的平均热膨胀系数为3.65×10- 6m/K。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，对于本领域的普通技术人员而言，在不脱离本发明的原理的情况下可以对这些实施例进行多种变化、修改、替换和变型，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。

Claims (10)

1.一种SiCf/SiC复合材料火焰筒的自动化制备方法，其特征在于，包括如下步骤：
1)将SiC纤维采用化学气相沉积法制备界面层，得到带连续界面层的SiC纤维；
2)根据仿真模拟计算得到的纤维体积和纤维走向，将步骤1)得到的带连续界面层的SiC纤维进行单向带铺放、缠绕成型，获得净尺寸成型的预制体；
3)对步骤2)得到的预制体先后采用反应熔体浸渗工艺和化学气相沉积工艺进行致密化处理，直至化学气相沉积工艺形成的SiC基体与反应熔体浸渗工艺形成的SiC基体的质量比为1～1∶2；
4)在步骤3)得到的预制体表面制备环境障碍涂层，所述环境障碍涂层的厚度为60～150um；
5)在步骤4)得到的预制体表面制备热障涂层，所述热障涂层的厚度为100～150um，全智能化得到高致密度SiCf/SiC复合材料火焰筒。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤1)中的界面层为PyC、SiC、B4C、ZrC、HfC、TaC、Si3N4、BN中的一种或多种。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤1)中，所述化学气相沉积工艺具体为：根据引入的界面层选择前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度为500～1400℃，沉积压力为0.5～12KPa，沉积时间为60～600min，沉积的界面层厚度为100nm～2μm；
所述前驱体为甲烷、三氯甲基硅烷、氯化硼、氯化锆、氯化钽、氯化硅、卤化硼、氨气中的一种或几种。
4.根据权利要求1所述的制备方法，其特征在于，所述步骤2)单向带铺带、缠绕成型包括如下步骤：
步骤一、使用丙酮清理火焰筒模具表面至无杂质附着状态，在火焰筒模具表面均匀涂覆2～3次的环氧树脂脱模剂，并对火焰筒模具加热到30～50℃；
步骤二、将体积含量为40～65％的SiC纤维、余量为树脂的预浸单向带分别铺覆在火焰筒模具的表面上；
步骤三、通过缠绕机将体积含量为50～70％的SiC纤维、余量为树脂的预浸单向带缠绕在步骤二铺设的模具表面上，由内向外以缠绕张力梯度递减的方式进行缠绕，缠绕角度为30～90°，缠绕速度为0.3～0.7m/s，缠绕张力为2～10N/cm，缠绕厚度为1～5mm；
步骤四、将经步骤三缠绕在模具表面上的材料层放入固化炉内固化成型，固化温度为90～165℃，固化时间为4～8h；
步骤五、将经步骤四固化成型后的预制体进行脱模，脱模后对预制体采用磨削加工及激光加工相结合方式进行产品精加工，即得到净尺寸成型的预制件。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤3)反应熔体浸渗工艺具体为熔融渗硅工艺：设备为真空高温气氛沉积炉和真空高温渗硅炉，以硅或硅合金为硅源，氩气为稀释气体，沉积温度为1400～1800℃，沉积压力为2Pa～常压，渗硅时间为30～300min；
所述硅合金为Si与Ta、Hf、Mo、W、Zr、Ti、B、Be的二元或三元的合金。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤3)的化学气相沉积工艺具体为，以三氯甲基硅烷为前驱体，氢气为反应气体，氩气为稀释气体，通过鼓泡法将气体引入到化学气相沉积炉中，沉积温度900～1200℃，沉积压力为0.5～5KPa，沉积时间为60～6000min。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤4)中的环境障碍涂层包括Si粘结层、稀土单硅酸盐Re2SiO5面层、以及位于所述粘结层和面层之间的Yb2Si2O7中间层；
所述Si粘结层、Yb2Si2O7中间层和稀土单硅酸盐Re2SiO5面层的厚度比为1～2：1～2：1～3；
所述稀土单硅酸盐Re2SiO5选自Y2SiO5、Sc2SiO5、Gd2SiO5、Er2SiO5、Tm2SiO5、Yb2SiO5、Lu2SiO5中的至少一种。
8.根据权利要求7所述的制备方法，其特征在于，所述环境障碍涂层的制备方法，包括以下步骤：
(1)对Yb2Si2O7和Re2SiO5分别进行球磨处理，直至粒径为20～80um；
(2)将预制件置于惰性保护气氛中，在1450～1800℃下热处理1～4h，形成Si粘结层；
(3)采用等离子体喷涂法，将Yb2Si2O7粉体喷涂在带有Si粘结层的预制件上，形成中间层；
(4)采用等离子体喷涂法，将稀土单硅酸盐Re2SiO5粉体喷涂在带有粘结层和中间层的预制件上，得到所述环境障碍涂层。
所述等离子喷涂法的参数包括：等离子气体包括氩气与氦气，所述氩气的流量为60～80slpm，所述氦气的流量为40～60slpm，送粉速率为10～35r/min，喷涂距离为90～200mm。
9.根据权利要求1所述的制备方法，其特征在于，所述步骤5)所述热障涂层为R2O3、ZrO2、CeO2、Al2O3·2SiO2、SrZrO3、La2Zr2O7、La2Ce2O7中的至少一种。
10.根据权利要求1～9任一项所述的方法制备得到的SiCf/SiC复合材料火焰筒。
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