CN112898024B - 一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件及其制备方法 - Google Patents

一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件及其制备方法 Download PDF

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CN112898024B
CN112898024B CN202110126624.8A CN202110126624A CN112898024B CN 112898024 B CN112898024 B CN 112898024B CN 202110126624 A CN202110126624 A CN 202110126624A CN 112898024 B CN112898024 B CN 112898024B
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刘海韬
孙逊
黄文质
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National University of Defense Technology
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Abstract

本发明涉及耐高温吸波结构领域，具体公开了一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件，所述构件自内至外依次包括：承载芯层、底层、吸波层、面层，所述承载芯层为连续碳纤维增强陶瓷基复合材料或连续低电阻率碳化硅纤维增强陶瓷基复合材料，所述底层和面层为高电阻率碳化硅纤维增强陶瓷基复合材料，所述吸波层为单层碳化硅纤维平纹布增强陶瓷基复合材料，各层复合材料陶瓷基体相同，为碳化硅、硅氧碳、硅碳氮、硅硼氮、氮化硼或硅硼碳氮中的一种。本发明还公开了吸波陶瓷翼舵类构件的制备方法。本发明提出的吸波陶瓷翼舵类构件具有高承载、抗烧蚀、强防热、宽频吸波等一体化功能，可显著提升新一代飞行器的生存与突防能力。

Description

一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件及其制备方法
技术领域
本发明属于耐高温吸波结构领域，特别涉及一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件及其制备方法。
背景技术
翼舵类部件是飞行器的重要组成部分，其主要起到控制飞行器稳定性、调控姿态等关键作用。同时，由于翼舵类构件雷达波散射特性显著，是飞行器上的强散射源之一，造成飞行器容易被探测打击，必须采用吸波材料技术降低其雷达波散射特性，提高生存与突防能力。随着飞行器速度的提升，翼舵类部件承受的热力载荷越来越大，对于高速飞行器而言，要求翼舵类构件具有防热/承载/抗烧蚀/吸波等一体化功能。现有高速飞行器翼舵类构件主要包括两种类型：金属芯层+树脂基复合材料防热外层和陶瓷基复合材料构件。
金属芯层+树脂基复合材料防热外层的吸波功能主要通过在树脂基复合材料防热外层中添加雷达吸收剂实现，但此类结构主要存在以下问题：1）吸收剂的添加会显著影响材料的均匀性，进而影响树脂基复合材料的力学和防热性能；2）吸收剂的添加会显著增加构件重量；3）吸收剂在复合材料中添加量有限，且受制于吸收剂的电磁参数频散特性，实现宽频吸波困难；4）此类构件对于高速长时的飞行器适用性差，高速长时飞行器的翼舵会承受严苛的热力载荷，树脂基复合材料防热外层会存在严重的烧蚀问题，造成翼舵外形发生明显变化，导致飞行器姿态控制与制导精度严重下降。陶瓷基复合材料构件具有防热、承载、抗烧蚀一体化功能，可以应用于热力载荷严苛的高速长时飞行器，由于载荷较大，目前此类构件主要采用具有高强特性的连续碳纤维增强碳化硅复合材料体系，但由于连续碳纤维的高电导率特性会对雷达波产生强散射，电磁散射特性与金属构件类似，因此不具备隐身功能。综上，现有技术方案均难以实现未来高速长时飞行器翼舵类构件的防热/承载/抗烧蚀/吸波等一体化功能，需要提出全新的技术方案。
发明内容
本发明的目的在于提供一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件，具备防热/承载/抗烧蚀/吸波等一体化功能，还提供了吸波陶瓷翼舵类构件的制备方法，从而克服背景技术中提到的不足与缺陷。
为实现上述目的，本发明提供了一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件，所述构件自内至外依次包括：承载芯层、底层、吸波层、面层，所述承载芯层为连续碳纤维增强陶瓷基复合材料或连续低电阻率碳化硅纤维增强陶瓷基复合材料，所述底层和面层为高电阻率碳化硅纤维增强陶瓷基复合材料，所述吸波层为单层碳化硅纤维平纹布增强陶瓷基复合材料，各层复合材料陶瓷基体相同，为碳化硅、硅氧碳、硅碳氮、硅硼氮、氮化硼或硅硼碳氮中的一种。
优选的，上述吸波陶瓷翼舵类构件中，所述连续碳纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳纤维织物，且织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，铜棒呈现正方形阵列排布，铜棒横纵方向轴心间距为10~15mm。
优选的，上述吸波陶瓷翼舵类构件中，所述连续低电阻率碳化硅纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳化硅纤维织物，所述碳化硅纤维电阻率低于0.1Ω·cm，且织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，铜棒呈现正方形阵列排布，铜棒横纵方向轴心间距为10~15mm。
优选的，上述吸波陶瓷翼舵类构件中，所述高电阻率碳化硅纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳化硅纤维织物，碳化硅纤维电阻率大于105Ω·cm，且纤维表面含有0.1~0.3μm厚度的氮化硼涂层。
优选的，上述吸波陶瓷翼舵类构件中，所述吸波层碳化硅纤维平纹布方阻为80~150Ω/sq，厚度为0.3~0.4mm。
一种上述的吸波陶瓷翼舵类构件的制备方法，包括以下步骤：
（1）将满足要求的碳纤维或碳化硅纤维按照构件设计尺寸预留余量制成纤维编织件，然后在织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，以碳化硅、硅氧碳、硅碳氮、硅硼氮、氮化硼或硅硼碳氮有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，完成承载芯层粗坯制备；
（2）根据承载芯层尺寸要求，按照设计尺寸对承载芯层粗坯进行机械加工，得到承载芯层；
（3）将承载芯层放入硝酸溶液中，将铜棒完全腐蚀掉，从而在承载芯层中形成缝合孔；将承载芯层用清水反复冲洗，直至清洗水无颜色且呈现中性，150℃条件下烘干2~4h；采用铜棒方式形成缝合孔，避免机械打孔对承载芯层造成损伤；
（4）制备满足厚度和电性能要求的底层碳化硅纤维编织件、面层碳化硅纤维编织件和吸波层碳化硅纤维平纹布；
（5）从承载芯层开始，在承载芯层两面对称层铺底层碳化硅纤维编织件、吸波层碳化硅纤维平纹布、面层碳化硅纤维编织件，调整位置采用编织工装固定，与承载芯层重叠区域采用碳化硅纤维通过承载芯层上的缝合孔缝合于承载芯层上，将非重叠区域的编织件采用碳化硅纤维缝合成为整体，完成构件编织件的制备；
（6）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，完成构件粗坯制备；
（7）将构件粗坯机械加工至设计尺寸；
（8）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对步骤（7）得到的构件粗坯继续进行浸渍、高温裂解和反复致密化，完成后致密化工作得到构件。
优选的，上述制备方法中，所述步骤（1）中，先驱体浸渍溶液中先驱体质量含量不低于40%；浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1200℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数不低于10次。
优选的，上述制备方法中，所述步骤（5）中，缝合所用碳化硅纤维的电阻率大于105Ω·cm；非重叠区域的纤维编织件缝合密度为4~16针/cm2。
优选的，上述制备方法中，所述步骤（6）中，浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1000℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数为6~8次。
优选的，上述制备方法中，所述步骤（8）中，浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1000℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数为3~4次。
与现有的技术相比，本发明具有如下有益效果：
1. 本发明提出了基于功能纤维梯度分布的吸波陶瓷翼舵类构件结构方式，可实现防热/承载/抗烧蚀/吸波一体化功能，以连续碳纤维增强陶瓷基复合材料或连续低电阻率碳化硅纤维增强陶瓷基复合材料为承载芯层，该材料具有耐高温、高强度特点，可以赋予翼舵类构件强的承载功能，同时低电阻率的承载芯层可以作为构件外层的雷达波反射背衬，增加雷达波在吸波层中的传输次数，增强吸波功能；电阻率梯度分布的碳化硅纤维增强陶瓷基复合材料具有耐高温、高强度、抗氧化、低热导特点，同时该材料可以在宽频段范围实现雷达波的阻抗匹配与损耗，具备宽频吸波功能。
2. 本发明的吸波陶瓷翼舵类构件中各层材料的热物理性能匹配性好，同时采用纤维缝合加后续致密化的工艺方式实现了一体化整体成型，具有整体性好，层间结合强度高、综合力学性能优异的优点。
3. 本发明提出的基于功能纤维梯度分布的翼舵类结构可以解决传统技术方案难题，可以应用于高速长时飞行器，具有高承载、抗烧蚀、强防热、宽频吸波等一体化功能，可显著提升新一代飞行器的生存与突防能力。
附图说明
图1是本发明中吸波陶瓷翼舵类构件的结构示意图。
图2是本发明实施例1中制备的承载芯层粗坯。
图3是本发明实施例1中制备的承载芯层粗坯加工后照片。
图4是本发明实施例1中制备的承载芯层铜棒腐蚀后照片。
图5是本发明实施例1中制备的构件编织件照片。
图6是本发明实施例1中制备的吸波陶瓷翼舵类构件照片。
主要附图标记说明：
1-承载芯层，2-底层，3-吸波层，4-面层。
具体实施方式
下面对本发明的具体实施方式进行详细描述，但应当理解本发明的保护范围并不受具体实施方式的限制。
实施例1
一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件，如图1所示，自内至外依次包括：连续碳纤维增强陶瓷基复合材料承载芯层1，高电阻率碳化硅纤维增强陶瓷基复合材料底层2（厚度2.5mm）、单层碳化硅纤维平纹布增强陶瓷基复合材料吸波层3、高电阻率碳化硅纤维增强陶瓷基复合材料面层4（厚度2.5mm），各层复合材料陶瓷基体均为碳化硅。连续碳纤维增强陶瓷基复合材料增强体为缝合碳纤维织物，且织物内植入直径1mm的铜棒，铜棒轴向与织物厚度方向平行，铜棒呈现正方形阵列排布，铜棒横纵方向轴心间距为10mm。高电阻率碳化硅纤维增强陶瓷基复合材料底层和面层中的增强体为缝合碳化硅纤维织物，碳化硅纤维电阻率为5×105Ω·cm，且纤维表面含有0.2μm厚度的氮化硼涂层。吸波层碳化硅纤维平纹布方阻为120Ω/sq，厚度为0.35mm。
本实施例还提供基于功能纤维梯度分布的吸波陶瓷翼舵类构件的制备方法，包括以下步骤：
（1）将满足要求的碳纤维按照构件设计尺寸预留余量制成纤维编织件，然后在织物内植入直径1mm铜棒，铜棒轴向与织物厚度方向平行，以聚碳硅烷二甲苯溶液为先驱体浸渍溶液，先驱体浸渍溶液中聚碳硅烷质量含量为50%，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，浸渍裂解工艺参数为：真空浸渍时间为6h，压力为-0.095MPa；高温裂解温度为1200℃，裂解气氛为高纯氮气，时间为0.5h；致密化12次，完成承载芯层粗坯（图2）制备；
（2）根据承载芯层尺寸要求，对承载芯层粗坯进行机械加工，使承载芯层尺寸满足要求，图3是承载芯层粗坯加工后照片；
（3）将承载芯层放入硝酸溶液中，将铜棒完全腐蚀掉，从而在承载芯层中形成缝合孔如图4所示；将承载芯层用清水反复冲洗，直至清洗水无颜色且呈现中性，150℃条件下烘干4h；
（4）制备满足厚度和电性能要求的底层碳化硅纤维编织件、面层碳化硅纤维编织件和吸波层碳化硅纤维平纹布；
（5）从承载芯层开始，在承载芯层两面对称层铺底层碳化硅纤维编织件、吸波层碳化硅纤维平纹布、面层碳化硅纤维编织件，调整位置采用编织工装固定，与承载芯层重叠区域采用电阻率为5×105Ω·cm的碳化硅纤维通过承载芯层上的缝合孔缝合于承载芯层上，将非重叠区域的编织件采用电阻率为5×105Ω·cm的碳化硅纤维缝合成为整体，非重叠区域的纤维编织件缝合密度为9针/cm2，完成构件编织件的制备，构件编织件如图5所述；
（6）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，浸渍裂解工艺参数为：真空浸渍时间为6h，压力为-0.095MPa；高温裂解温度为900℃，裂解气氛为高纯氮气，时间为1h；致密化8次，完成构件粗坯制备；
（7）将构件粗坯机械加工至设计尺寸；
（8）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对步骤（7）得到的构件粗坯继续进行浸渍、高温裂解和反复致密化，浸渍裂解工艺参数为：真空浸渍时间为6h，压力为-0.095MPa；高温裂解温度为900℃，裂解气氛为高纯氮气，时间为1h；致密化4次，得到吸波陶瓷翼舵类构件。
图6为本实施例制备的吸波陶瓷翼舵类构件照片，该构件具有优异的高承载、强防热、宽频吸波等一体化功能，C、X、Ku频段雷达散射特性相对金属可减小8dB以上。
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式，并且很显然，根据上述教导，可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用，从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。

Claims (6)

1.一种基于功能纤维梯度分布的吸波陶瓷翼舵类构件的制备方法，其特征在于，所述构件自内至外依次包括：承载芯层、底层、吸波层、面层，所述承载芯层为连续碳纤维增强陶瓷基复合材料或连续低电阻率碳化硅纤维增强陶瓷基复合材料，所述底层和面层为高电阻率碳化硅纤维增强陶瓷基复合材料，所述吸波层为单层碳化硅纤维平纹布增强陶瓷基复合材料，各层复合材料陶瓷基体相同，为碳化硅、硅氧碳、硅碳氮、硅硼氮、氮化硼或硅硼碳氮中的一种；所述连续低电阻率碳化硅纤维增强陶瓷基复合材料中碳化硅纤维电阻率低于0.1Ω·cm，且所述高电阻率碳化硅纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳化硅纤维织物，碳化硅纤维电阻率大于105Ω·cm；且纤维表面含有0.1~0.3μm厚度的氮化硼涂层；所述吸波层碳化硅纤维平纹布方阻为80~150Ω/sq，厚度为0.3~0.4mm；
所述吸波陶瓷翼舵类构件的制备方法，包括以下步骤：
（1）将满足要求的碳纤维或碳化硅纤维按照构件设计尺寸预留余量制成纤维编织件，然后在织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，以碳化硅、硅氧碳、硅碳氮、硅硼氮、氮化硼或硅硼碳氮有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，完成承载芯层粗坯制备；
（2）根据承载芯层尺寸要求，按照设计尺寸对承载芯层粗坯进行机械加工，得到承载芯层；
（3）将承载芯层放入硝酸溶液中，将铜棒完全腐蚀掉，从而在承载芯层中形成缝合孔；将承载芯层用清水反复冲洗，直至清洗水无颜色且呈现中性，150℃条件下烘干2~4h；
（4）制备满足厚度和电性能要求的底层碳化硅纤维编织件、面层碳化硅纤维编织件和吸波层碳化硅纤维平纹布；
（5）从承载芯层开始，在承载芯层两面对称层铺底层碳化硅纤维编织件、吸波层碳化硅纤维平纹布、面层碳化硅纤维编织件，调整位置采用编织工装固定，与承载芯层重叠区域采用碳化硅纤维通过承载芯层上的缝合孔缝合于承载芯层上，将非重叠区域的编织件采用碳化硅纤维缝合成为整体，完成构件编织件的制备；缝合所用碳化硅纤维的电阻率大于105Ω·cm，非重叠区域的纤维编织件缝合密度为4~16针/cm2；
（6）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对纤维编织件进行浸渍、高温裂解和反复致密化，完成构件粗坯制备；
（7）将构件粗坯机械加工至设计尺寸；
（8）以步骤（1）相同的有机先驱体溶液为浸渍溶液，采用先驱体浸渍裂解工艺对步骤（7）得到的构件粗坯继续进行浸渍、高温裂解和反复致密化，完成后致密化工作得到构件。
2.根据权利要求1所述的制备方法，其特征在于，所述连续碳纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳纤维织物，且织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，铜棒呈现正方形阵列排布，铜棒横纵方向轴心间距为10~15mm。
3.根据权利要求1所述的制备方法，其特征在于，所述连续低电阻率碳化硅纤维增强陶瓷基复合材料增强体为针刺、缝合、2.5D、3D碳化硅纤维织物，且织物内植入直径1~1.2mm的铜棒，铜棒轴向与织物厚度方向平行，铜棒呈现正方形阵列排布，铜棒横纵方向轴心间距为10~15mm。
4.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，先驱体浸渍溶液中先驱体质量含量不低于40%；浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1200℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数不低于10次。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤（6）中，浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1000℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数为6~8次。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤（8）中，浸渍裂解工艺参数为：真空浸渍时间不低于4h，压力不大于-0.09MPa；高温裂解温度为800~1000℃，裂解气氛为惰性气氛，时间为0.5~1h；致密化次数为3~4次。
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CN103922776B (zh) * 2014-04-01 2015-09-02 中国人民解放军国防科学技术大学 碳化硅纤维增强碳化硅复合材料吸波陶瓷及其制备方法
CN106218061B (zh) * 2016-07-26 2018-02-09 中国人民解放军国防科学技术大学 一种双层结构陶瓷基复合材料及其制备方法

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