WO2022007377A1 - 一种混编纤维预制体增强的复合材料及其制备方法 - Google Patents

一种混编纤维预制体增强的复合材料及其制备方法 Download PDF

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Publication number
WO2022007377A1
WO2022007377A1 PCT/CN2021/070325 CN2021070325W WO2022007377A1 WO 2022007377 A1 WO2022007377 A1 WO 2022007377A1 CN 2021070325 W CN2021070325 W CN 2021070325W WO 2022007377 A1 WO2022007377 A1 WO 2022007377A1
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Prior art keywords
fiber
composite material
preform
matrix
fibers
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PCT/CN2021/070325
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English (en)
French (fr)
Inventor
陈照峰
肖七巧
缪云良
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Priority to US17/431,206 priority Critical patent/US20220194863A1/en
Publication of WO2022007377A1 publication Critical patent/WO2022007377A1/zh
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Definitions

  • the invention relates to a composite material and a preparation method thereof, in particular to a composite material reinforced by a mixed fiber preform and a preparation method thereof.
  • the fiber preform is used as the reinforcing structure of the composite material, and the external load is transferred to the fiber through the matrix.
  • the fiber preform is an important guarantee for the structural strength of the composite material.
  • the fiber preform is composed of a single fiber, which usually has the problems of limited reinforcement effect, high cost, and single function.
  • the use of mixed fiber preform can effectively solve the above problems. To further meet the needs of high temperature resistance, heat insulation, wave absorption and other functions.
  • the Chinese utility model patent with the application announcement number CN206173595U discloses an aramid fiber blended fabric, which consists of four layers in total, which are layered from top to bottom, namely: the glass fiber warp yarn layer in the 0° direction, the -45° direction
  • the aramid layer, the aramid layer in the +45° direction, and the surface felt of the bottom layer, the above four-layer structures are laid in sequence, and then stitched together with stitching threads to form a aramid fiber blended fabric.
  • the utility model patent mixes glass fiber and aramid fiber, and the obtained mixed braid solves the problems of high rigidity, insufficient toughness and poor impact resistance of a single glass fiber reinforced plastic composite material, and at the same time, the strength is greatly increased.
  • the Chinese invention patent with the application publication number CN106868676B discloses a three-dimensional hybrid polyimide fiber reinforced polyoxymethylene composite material and a preparation method thereof.
  • polyimide fibers and polyoxymethylene fibers are made into covered yarns, and then woven to obtain a three-dimensional mixed braid, and the mixed braid is molded into a composite material.
  • the method is simple in process, can prepare polyimide fiber reinforced polyoxymethylene composite materials with different structures, and ensures that the reinforcing fibers obtain effective length, are fully impregnated, and are uniformly dispersed in the matrix.
  • the improvement effect of formaldehyde strength and modulus is provided.
  • the Chinese invention patent with application publication number CN110845826A discloses a preparation method of a silk-based impact-resistant hybrid fiber composite material, the steps are as follows: selecting mulberry/tussah silk fabric and carbon fiber/flax fiber fabric; weaving of interlayer mixed fabric; Pretreatment of reinforcement fabrics; Hybrid fiber fabric reinforced epoxy resin composites were prepared by hand lay-up + hot pressing molding process and vacuum resin transfer molding process.
  • the preparation process of the invention is simple, the final product has high performance stability, can improve the fracture toughness and impact toughness of the carbon fiber composite material, and is an impact-resistant composite material with application prospects.
  • the fiber preforms studied are mostly composed of organic fibers, the fibers are flexible, the textile performance is good, and the process is simple, and there is a lack of high-performance inorganic fiber blended preform products.
  • the current research focuses on the mechanical properties of resin-based composites, and there are few studies on the properties of ceramics, metal matrices, and composites such as high temperature resistance, ablation resistance, and wave absorption. Therefore, the development of high-performance inorganic fiber blended fiber preform reinforced composites has important application value.
  • the present invention proposes a composite material reinforced by a mixed fiber preform, which improves the composition and structure of the existing mixed fiber preform, thereby overcoming the shortcomings of the existing materials and technologies.
  • the present invention provides a composite material reinforced by a mixed fiber preform, which is composed of a fiber preform, a composite material interface and a matrix, and the fiber preform is a three-dimensional three-dimensional woven by 2 to 5 kinds of fibers.
  • the fiber volume fraction in the fiber preform is 35% to 65%
  • the volume fraction of a single fiber in the preform is 5% to 60%
  • the number of layers of fiber cloth or felt in the preform is 2 to 5 layers
  • the thickness of each layer is 0.5-50mm
  • the three-dimensional overall structure is formed by needle stitching, resin bonding, yarn feeding and shallow cross-linking between the layers.
  • the fibers are woven by loom temples during the weaving process;
  • the outer layer of the composite material is quartz fiber, and the inner layer is high silica fiber or glass fiber;
  • the outer layer of the absorbing composite material is oxide fiber, the middle layer is silicon carbide fiber, and the inner layer is carbon fiber;
  • the outer layer of high temperature structural material is silicon carbide Fiber, the inner layer is carbon fiber;
  • the outer layer of the thermal insulation composite material below 1400 °C is silicon carbide fiber, the middle layer is carbon fiber, alumina fiber, and the inner layer is glass fiber;
  • the outer layer of the thermal insulation composite material above 1400 °C is carbon fiber, and the middle layer is carbon fiber.
  • the layers are silicon carbide fibers, alumina fibers, and quartz fibers in sequence, and the inner layer is high-silica fibers; the fiber cloth or felt used is composed of 1 to 3 kinds of fibers and 0 to 3 kinds of ceramic powders, and the fiber cloth or felt is composed of ceramic powder.
  • the volume fraction of the powder is 0-30%
  • the volume fraction of the binder in the ceramic powder is 0-5%
  • the ceramic powder is silicon carbide, boron carbide, zirconium carbide, tantalum carbide, hafnium carbide, silicon nitride, Boron nitride, silicon oxide, calcium oxide, yttrium oxide, zirconium oxide and aluminum oxide
  • the interface is fullerene
  • graphene pyrolytic carbon
  • silicon carbide boron nitride and oxide interface
  • the matrix material is Resins, light alloys, carbon and ceramics.
  • the preparation method of the above-mentioned mixed fiber preform reinforced composite material adopts the following sequential steps:
  • Step 1 preparing ceramic slurry, adjusting the Zeta potential of the slurry, and ball milling to form a stable suspension
  • Step 2 dipping the fiber bundle in the ceramic slurry, and then pulling it out from the slurry to maintain the ceramic content in the fiber bundle;
  • Step 3 winding, laying, and weaving the fiber impregnating material into a two-dimensional cloth, or a three-dimensional thin-walled structure, and the fibers are weaved by a loom temple during the weaving process;
  • Step 4 stacking two-dimensional fabrics of different fiber types, or nesting three-dimensional thin-walled structures of different fibers;
  • Step 5 forming a three-dimensional overall structure preform by means of needle stitching, resin bonding, yarn feeding and shallow cross-linking between layers;
  • Step 6 treating the preform at 300-1000°C under vacuum or inert atmosphere
  • Step 7 preparing the interface for the prefab
  • a ceramic matrix is prepared by impregnation and pyrolysis of a precursor to obtain a ceramic matrix composite material; a resin matrix is prepared by impregnation with resin transfer molding to obtain a resin matrix composite material; an alloy matrix is prepared by vacuum pressure impregnation to obtain a metal matrix composite material.
  • the present invention has the following beneficial effects: (1) effectively solve the problem that the fibers are easy to produce filaments during the weaving process, and improve the knitability of the fibers; (2) the integrity of the mixed fiber preform is good, The bonding strength between layers is high, and it is not easy to delaminate; (3) the densification period of the composite material is short, the fiber damage is small, the structure strength is high, and the integration of structure and function is realized; (4) the multi-layer design on the structure reduces the usage of high-priced fibers .
  • a composite material reinforced by a mixed fiber preform is composed of a fiber preform, a composite material interface and a matrix.
  • the fiber preform is a three-dimensional three-dimensional fabric woven by three kinds of fibers, and the fiber volume fraction in the fiber preform is 35.
  • the outer layer is a glass fiber wave-transmitting layer, the glass fiber volume fraction is 10%, the thickness is 5mm, the plain weave is used, and its impedance is about 400 ⁇ , the middle layer is a silicon carbide fiber loss layer, and the volume fraction of silicon carbide fibers It is 15%, the thickness is 3mm, the plain weave is adopted, the resistivity is 1-10 ⁇ cm, the dielectric loss tangent value is 0.6, the inner layer is a carbon fiber reflective layer, the carbon fiber volume fraction is 10%, the thickness is 0.8mm, and the fabric structure It is a satin texture, the resistivity is ⁇ 0.5 ⁇ cm, and the impedance of each layer gradually decreases from the outside to the inside; the middle layer fiber cloth used is composed of silicon carbide fibers and silicon carbide ceramic powder, and the volume
  • the preparation method of the above-mentioned mixed fiber preform reinforced composite material adopts the following sequential steps:
  • Step 1 prepare silicon carbide ceramic slurry, adjust the Zeta potential of the slurry to 50mV, and ball mill to form a stable suspension;
  • Step 2 dipping the glass fiber bundles, silicon carbide fiber bundles, and carbon fiber bundles in the ceramic slurry, then pulling them out from the slurry, maintaining the ceramic content in the fiber bundles, and drying at 80° C. for 10 hours;
  • Step 3 weaving the glass fiber into a two-dimensional plain weave, weaving the silicon carbide fiber into a two-dimensional plain weave, and weaving the carbon fiber into a two-dimensional 2/2 satin weave.
  • the warp density is 6.0 pieces/cm
  • the silicon carbide ceramic powder is added when weaving the silicon carbide fiber cloth, and the areal density of the ceramic powder is 200 g/m 2 ;
  • Step 4 stacking the obtained glass fiber cloth, silicon carbide fiber cloth, and carbon fiber cloth in turn;
  • Step 5 the three-dimensional overall structure preform is formed between the layers by adding yarn and threading;
  • Step 6 treating the preform at 700°C under vacuum, keeping the temperature for 1 hour;
  • Step 7 using silica sol as a precursor, vacuum impregnation with an external pressure of 0.5 MPa, dehydration and gelation at 90° C. for 12 hours, and heat treatment at 750° C. for 2 hours to prepare a silica interface;
  • step 8 a silicon carbide ceramic matrix is prepared by impregnation with silica sol.
  • the operation steps are the same as in step 7, and the impregnation is repeated for 12 cycles to obtain a ceramic matrix composite material.
  • the prepared composite materials have a dielectric loss tangent value of 0.3-0.6 in the 8.2-18.0GHz frequency band of electromagnetic waves.
  • Table 1 shows the specific wave-absorbing properties and mechanical properties of the materials.
  • the highest reflectivity in the X-band can reach -20.1dB.
  • the flexural strength of the composite material can reach 301MPa. Due to its excellent absorbing performance and flexural strength, it has important application value in the field of structural absorbing.
  • a composite material reinforced by a mixed fiber preform is composed of a fiber preform, a composite material interface and a matrix.
  • the fiber preform is a three-dimensional three-dimensional fabric woven by two kinds of fibers, and the fiber volume fraction in the preform is 45%.
  • the number of layers of fiber cloth in the fiber preform is 2 layers, and the three-dimensional overall structure is formed by needle stitching between the layers.
  • the fiber is woven by the loom temple during the weaving process;
  • the fiber preform is a high-temperature structural material: external
  • the layer is silicon carbide fiber, the volume fraction of silicon carbide fiber in the fiber preform is 15%, the thickness is 8mm, the inner layer is carbon fiber, the volume fraction of carbon fiber is 20%, and the thickness is 12mm;
  • the fiber cloth used is composed of silicon carbide fiber and carbon fiber respectively. It is composed of one kind of ceramic powder, the volume fraction of ceramic powder in the fiber cloth is 3%, the volume fraction of binder in the ceramic powder is 1%, the ceramic powder used is silicon carbide, the interface is pyrolytic carbon interface, and the matrix is The material is silicon carbide ceramics.
  • the preparation method of the above-mentioned mixed fiber preform reinforced composite material adopts the following sequential steps:
  • Step 1 prepare silicon carbide ceramic slurry, adjust the Zeta potential of the slurry to 60mV, and ball mill to form a stable suspension;
  • Step 2 the fiber bundles of silicon carbide and carbon fibers are dipped in the silicon carbide ceramic slurry, and then pulled out from the slurry, maintaining the ceramic content in the fiber bundles, and drying at 70°C for 12 hours;
  • Step 3 weaving the treated carbon fiber and silicon carbide fiber impregnating material into a three-dimensional thin-walled structure, the fabric type is a shallow cross-linked fabric, the fibers are woven by loom temples during the weaving process, and silicon carbide ceramics are added during the weaving process.
  • Step 4 nesting the three-dimensional thin-walled structures of carbon fibers and silicon carbide fibers
  • Step 5 the layers of the nested preforms are formed by needle stitching to form a three-dimensional overall structure preform
  • Step 6 treating the preform in vacuum at 1000°C for 1 hour;
  • Step 7 prepare the pyrolytic carbon interface by chemical vapor deposition, the gas source used is propylene, the diluent gas is nitrogen, the total system pressure is 10kPa, the P N2 /P C3H6 is 2:1, the deposition temperature is 900 ° C, and the deposition time is 2 hours .
  • Step 8 prepare silicon carbide ceramic matrix by precursor impregnation and pyrolysis, use polycarbosilane as precursor and xylene as solvent to prepare precursor solution, vacuum impregnation, and then pyrolyze at 1000°C for 1 hour, repeating 11 cycles of impregnation and pyrolysis , to obtain ceramic matrix composites.
  • the density of the prepared composite material is lower than 2.6 g/cm 3 , the high temperature resistance performance is good, up to 1200° C., the flexural strength at high temperature can reach 280 MPa, and the oxidation resistance performance is excellent.
  • a composite material reinforced by a mixed fiber preform is composed of a fiber preform, a composite material interface and a matrix.
  • the fiber preform is a three-dimensional three-dimensional fabric woven by 5 kinds of fibers, and the volume fraction of the fiber in the fiber preform is: 65%, the number of layers of fiber cloth in the fiber preform is 5 layers, the thickness of each layer is 10-50mm, the layers are bonded by resin to form a three-dimensional overall structure, and the fibers are woven by loom temples during the weaving process.
  • the fiber preform is a heat-resistant composite material above 1400°C: the outer layer is carbon fiber, the volume fraction of carbon fiber is 15%, and the thickness is 10mm; The volume fractions are 10%, 10%, and 10%, respectively, and the thicknesses are 8mm, 8mm, and 8mm, respectively.
  • 1 type of fiber and 0 or 1 type of ceramic powder the volume fraction of ceramic powder in the fiber cloth is 5%, the volume fraction of the binder in the ceramic powder is 3%, and silicon nitride is added to the silicon carbide fiber layer Ceramic powder, alumina fiber, quartz fiber and high silica fiber are added with alumina ceramic powder, the interface is a silicon carbide interface, and the matrix material is ceramic.
  • the preparation method of the above-mentioned mixed fiber preform reinforced composite material adopts the following sequential steps:
  • Step 1 prepare silicon nitride ceramic slurry, adjust the Zeta potential of the slurry to 30mV, and ball mill to form a stable suspension;
  • Step 2 Impregnate carbon fiber bundles, silicon carbide fiber bundles, alumina fiber bundles, quartz fiber bundles, and high-silica fiber bundles in the ceramic slurry, and then pull them out from the slurry to maintain the ceramic content in the fiber bundles at 80°C dry for 12 hours;
  • Step 3 Weaving the obtained fiber impregnating materials into a three-dimensional thin-walled structure, the fibers are weaved by loom temples during the weaving process, wherein the warp density of carbon fibers and silicon carbide is 6.0 pieces/cm, and nitrogen is added during the weaving process.
  • Silicon ceramic powder, the areal density of ceramic powder is 200g/m 2
  • the warp density of alumina fiber, quartz fiber and high silica fiber is 8.0 pieces/cm
  • alumina powder is added during the weaving process
  • the areal density of ceramic powder is 180g /m 2 ;
  • Step 4 nesting the obtained three-dimensional thin-walled structures of carbon fibers, silicon carbide fibers, alumina fibers, quartz fibers, and high-silica fibers in sequence;
  • Step 5 forming a three-dimensional overall structure preform by resin bonding between layers
  • Step 6 treating the preform at 700°C for 1 hour under an argon atmosphere
  • Step 7 preparing a silicon carbide interface by chemical vapor deposition, using tetrachlorosilane and methane as source substances, the deposition temperature is 500°C, and the deposition time is 1 hour;
  • Step 8 For the outer layer of carbon fibers, prepare a carbon matrix by chemical vapor deposition, and for the remaining layers, prepare a silica matrix by impregnation with silica sol. Microspheres or phenolic glass microspheres, the content of microspheres is less than 10%, dehydrated and gelled at 85°C for 10 hours, then heat-treated at 750°C for 1 hour, and repeated immersion and pyrolysis for 10 cycles to obtain a ceramic matrix composite material.
  • the above-mentioned composite materials prepared can be used at a temperature of up to 1400 ° C, the thermal expansion coefficient of the material is less than 4.5 ⁇ 10 -6 / ° C, the thermal conductivity is less than 40 W/m ⁇ K, and the ablation resistance is good.
  • the layer temperature difference is higher than 700 °C, which effectively realizes the integration of heat protection and heat insulation.

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Abstract

一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，其中纤维预制体是由2～5种高性能无机纤维混编而成的三维立体织物，基体为树脂、轻合金、碳和陶瓷。该复合材料的制备方法包括：制备陶瓷浆料、纤维束浸浆处理、纤维编织、三维整体结构预制体成型、预制体热处理、界面制备和基体制备。

Description

一种混编纤维预制体增强的复合材料及其制备方法
本申请要求于2020年07月09日提交中国专利局、申请号为202010683522.1、发明名称为“一种混编纤维预制体增强的复合材料及其制备方法”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及一种复合材料及其制备方法，尤其涉及一种混编纤维预制体增强的复合材料及其制备方法。
背景技术
连续纤维高性能高强度赋予其增强的复合材料轻质、高强、多功能等众多优点，是当前材料领域内最具应用潜力的材料之一，但是受限于复合材料内部结构和纤维种类的单一性，其应用范围受到一定限制。因此，通过复合材料纤维增强体的结构设计，开发结构强度和功能一体化的混编纤维预制体及复合材料十分必要。
纤维预制体作为复合材料的增强结构，外部载荷经由基体传递到纤维上，纤维预制体是复合材料结构强度的重要保证。传统条件下，纤维预制体由单种纤维组成，通常会存在增强效果有限、成本较高、功能单一的问题，使用混编纤维预制体可以有效地解决上述问题，同时可通过纤维和基体的选择进一步满足对耐高温、防隔热、吸波等功能的需求。
申请公告号为CN206173595U的中国实用新型专利公告了一种芳纶纤维混编织物，总共包含四层结构，从上到下层叠铺设，分别为：0°方向的玻纤经纱层、-45°方向的芳纶层、+45°方向的芳纶层以及底层的表面毡，上述四层结构顺序铺放，然后利用缝编线缝合在一起，组成芳纶纤维混编织物。该实用新型专利将玻璃纤维与芳纶纤维进行混编，得到的混编织物解决了单一的玻璃钢复合材料刚性大而韧性不足、耐冲击性差的问题，同时在强度方面得到了大幅度的增加。
申请公告号为CN106868676B的中国发明专利公开了一种三维混编聚酰亚胺纤维增强聚甲醛复合材料及其制备方法。该发明将聚酰亚胺纤维 与聚甲醛纤维制成包覆纱，再进行编织得到三维混编织物，混编织物经模压制成复合材料。该方法工艺简单，可制备不同结构的聚酰亚胺纤维增强聚甲醛复合材料，保证增强纤维获取有效长度、得到充分浸渍、在基体内均匀分散，纤维添加量极高，最大程度发挥纤维对聚甲醛强度、模量的改善效果。
申请公开号为CNl10845826A的中国发明专利公开了一种基于蚕丝的抗冲击混杂纤维复合材料的制备方法，步骤如下：挑选桑/柞蚕丝织物与碳纤维/亚麻纤维织物；层内混编织物的编织；增强体织物的预处理；手糊+热压成型工艺及真空树脂传递模塑成型工艺制备混杂纤维织物增强环氧树脂复合材料。该发明制备工艺简易，最终成品性能稳定性高，可提升碳纤维复合材料的断裂韧性和冲击韧性，是一种具有应用前景的抗冲击复合材料。
目前，由于所研究的纤维预制体多为有机纤维组成，纤维柔性大，纺织性能好，工艺简单，对高性能的无机纤维混编预制体产品缺乏。此外，对于混编纤维预制体增强的复合材料，当前研究以树脂基复合材料的力学性能为主，对陶瓷、金属基体以及复合材料的耐高温、耐烧蚀、吸波等性能研究较少，所以，开发高性能无机纤维混编纤维预制体增强复合材料有重要的应用价值。
发明内容
为解决上述问题，本发明提出一种混编纤维预制体增强的复合材料，对现有的混编纤维预制体的组成和结构进行了改进，从而克服现有材料及技术的缺点。
为实现上述目的，本发明提供一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，所述纤维预制体为由2～5种纤维编织而成的三维立体织物，所述纤维预制体中纤维体积分数为35％～65％，预制体中单种纤维的体积分数为5％～60％，预制体中纤维布或毡的层数为2～5层，各层厚度0.5～50mm，层与层之间通过针刺缝合、树脂粘结、加纱引纱和浅交弯联方式形成三维整体结构，纤维在编织过程中采用织机边撑织造；透波复合材料外层为石英纤维，内层为高硅氧纤维或玻璃纤维；吸波复合材料外层为氧化物纤维，中间层为碳化硅纤维，内 层为碳纤维；高温结构材料外层为碳化硅纤维，内层为碳纤维；1400℃以下隔热复合材料外层为碳化硅纤维，中间层依次为碳纤维、氧化铝纤维，内层为玻璃纤维；1400℃以上防热复合材料外层为碳纤维，中间层依次为碳化硅纤维、氧化铝纤维、石英纤维，内层为高硅氧纤维；采用的纤维布或毡由1～3种纤维与0～3种陶瓷粉体组成，纤维布或毡中陶瓷粉体体积分数为0～30％，陶瓷粉体中粘结剂体积分数为0～5％，所述陶瓷粉体为碳化硅、碳化硼、碳化锆、碳化钽、碳化铪、氮化硅、氮化硼、氧化硅、氧化钙、氧化钇、氧化锆和氧化铝，所述界面为富勒烯、石墨烯、热解碳、碳化硅、氮化硼和氧化物界面，所述基体材料为树脂、轻合金、碳和陶瓷。
上述混编纤维预制体增强的复合材料的制备方法采用以下顺序步骤：
步骤1，制备陶瓷浆料，调整浆料Zeta电位，球磨形成稳定悬浮液；
步骤2，将纤维束在陶瓷浆料中浸渍，然后从浆料中拉出，保持纤维束中陶瓷含量；
步骤3，将纤维浸渍料缠绕、铺层、编织成二维布，或三维薄壁结构，纤维在编织过程中采用织机边撑织造；
步骤4，将不同纤维种类的二维布叠加，或不同纤维的三维薄壁结构嵌套；
步骤5，层与层之间针刺缝合、树脂粘结、加纱引纱和浅交弯联方式形成三维整体结构预制体；
步骤6，对预制体真空或惰性气氛下300～1000℃处理；
步骤7，对预制体制备界面；
步骤8，通过先驱体浸渍热解制备陶瓷基体，得到陶瓷基复合材料；通过树脂传递模塑浸渍制备树脂基体，得到树脂基复合材料；通过真空压力浸渍制备合金基体，得到金属基复合材料。
与现有材料及技术相比，本发明具有如下有益效果：(1)有效解决编织过程纤维易产生毛丝的问题，提高纤维的可编织性；(2)混编纤维预制体整体性好，层间结合强度高，不易分层；(3)复合材料致密化周期短，纤维损伤小结构强度高，实现结构功能一体化；(4)结构上多层设计减小了高价格纤维的使用量。
具体实施方式
下面结合具体实施例，进一步阐明本发明，应理解这些实施例仅用于说明本发明而不用于限制本发明的范围，在阅读了本发明之后，本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，所述纤维预制体由3种纤维编织而成的三维立体织物，纤维预制体中纤维体积分数为35％，纤维预制体中纤维布层数为3层，层与层之间通过加纱引纱的方式形成三维整体结构，纤维在编织过程中采用织机边撑织造；所述纤维预制体为吸波复合材料：外层为玻璃纤维透波层，玻璃纤维体积分数为10％，厚度为5mm，采用平纹组织，其阻抗约为400Ω，中间层为碳化硅纤维损耗层，碳化硅纤维的体积分数为15％，厚度为3mm，采用平纹组织，电阻率为1～10Ω·cm，介电损耗正切值为0.6，内层为碳纤维反射层，碳纤维体积分数为10％，厚度为0.8mm，织物组织为缎纹组织，电阻率<0.5Ω·cm，从外至里，各层阻抗逐渐递减；采用的中间层纤维布由碳化硅纤维与碳化硅陶瓷粉体组成，纤维布中陶瓷粉体体积分数为5％，陶瓷粉体中粘结剂体积分数为2％，采用的界面为二氧化硅界面，基体材料为二氧化硅。
上述混编纤维预制体增强的复合材料的制备方法采用以下顺序步骤：
步骤1，制备碳化硅陶瓷浆料，调整浆料Zeta电位至50mV，球磨形成稳定悬浮液；
步骤2，将玻璃纤维纤维束、碳化硅纤维束、碳纤维束在陶瓷浆料中浸渍，然后从浆料中拉出，保持纤维束中陶瓷含量，80℃保温10小时干燥；
步骤3，将玻璃纤维编织成二维平纹布、将碳化硅纤维编织成二维平纹布、将碳纤维编织成二维2/2缎纹布，纤维在编织过程中采用织机边撑织造，编织过程中经纱密度为6.0根/cm，其中在编织碳化硅纤维布时加入碳化硅陶瓷粉，陶瓷粉末的面密度为200g/m 2；
步骤4，将得到的玻璃纤维布、碳化硅纤维布、碳纤维布依次叠加；
步骤5，层与层之间通过加纱引纱方式形成三维整体结构预制体；
步骤6，对预制体真空下700℃处理，保温1小时；
步骤7，以硅溶胶为先驱体，外加压力0.5MPa进行真空浸渍，在90℃保温12小时脱水凝胶化，750℃保温2小时进行热处理，制备二氧化硅界面；
步骤8，通过硅溶胶浸渍制备碳化硅陶瓷基体，操作步骤同步骤7，重复浸渍12个周期，得到陶瓷基复合材料。
制备的上述复合材料在8.2-18.0GHz频段电磁波的介电损耗正切值为0.3～0.6，表1为材料的具体吸波性能和力学性能参数，在X波段的最高反射率可达-20.1dB，复合材料的弯曲强度可达301MPa，由于吸波性能和弯曲强度表现优异，在结构吸波领域有重要应用价值。
表1混编纤维预制体增强的碳化硅陶瓷基吸波材料的吸波性能和力学性能
Figure PCTCN2021070325-appb-000001
实施例2
一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，所述纤维预制体由2种纤维编织而成的三维立体织物，预制体中纤维体积分数为45％，纤维预制体中纤维布的层数为2层，层与层之间通过针刺缝合方式形成三维整体结构，纤维在编织过程中采用织机边撑织造；纤维预制体为高温结构材料：外层为碳化硅纤维，纤维预制体中碳化硅纤维体积分数15％，厚度为8mm，内层为碳纤维，碳纤维的体积分数为20％，厚度为12mm；采用的纤维布分别由碳化硅纤维、碳纤维与1种陶瓷粉体组成，纤维布中陶瓷粉体体积分数为3％，陶瓷粉体中粘结剂体积分数为1％，采用的陶瓷粉体为碳化硅，界面为热解碳界面，基体材料为碳化硅陶瓷。
上述混编纤维预制体增强的复合材料的制备方法采用以下顺序步骤：
步骤1，制备碳化硅陶瓷浆料，调整浆料Zeta电位至60mV，球磨形成稳定悬浮液；
步骤2，将碳化硅和碳纤维的纤维束在碳化硅陶瓷浆料中浸渍，然后 从浆料中拉出，保持纤维束中陶瓷含量，70℃保温12小时干燥；
步骤3，将处理过的碳纤维和碳化硅纤维浸渍料编织成三维薄壁结构，织物类型为浅交弯联织物，纤维在编织过程中采用织机边撑织造，在编织过程中加入碳化硅陶瓷粉末，其中碳化硅粉末的面密度为225g/m 2；
步骤4，将碳纤维和碳化硅纤维的三维薄壁结构嵌套；
步骤5，嵌套的预制体的层与层之间通过针刺缝合方式形成三维整体结构预制体；
步骤6，对预制体真空1000℃处理1小时；
步骤7，通过化学气相沉积制备热解碳界面，使用的气源为丙烯，稀释气体为氮气，系统总压为10kPa，P N2/P C3H6为2：1，沉积温度900℃，沉积时间2小时。
步骤8，通过先驱体浸渍热解制备碳化硅陶瓷基体，以聚碳硅烷为先驱体、二甲苯为溶剂制备先驱体溶液，真空浸渍，然后1000℃热解1小时，重复浸渍热解11个周期，得到陶瓷基复合材料。
制备的上述复合材料的密度低于2.6g/cm 3，耐高温性能好，高达1200℃，高温下抗弯强度可达280MPa，抗氧化性能优异。
实施例3
一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，所述纤维预制体由5种纤维编织而成的三维立体织物，纤维预制体中纤维的体积分数为65％，纤维预制体中纤维布的层数为5层，各层的厚度为10～50mm，层与层之间通过树脂粘结形成三维整体结构，纤维在编织过程中采用织机边撑织造；所述纤维预制体为1400℃以上防热复合材料：外层为碳纤维，碳纤维的体积分数为15％，厚度为10mm；中间层依次为碳化硅纤维、氧化铝纤维、石英纤维，各纤维的体积分数分别为10％、10％、10％，厚度分别为8mm、8mm、8mm，内层为高硅氧纤维，高硅氧纤维的体积分数为20％，厚度为10mm；采用的纤维布由1种纤维与0或1种陶瓷粉体组成，纤维布中陶瓷粉体的体积分数为5％，陶瓷粉体中粘结剂的体积分数为3％，其中碳化硅纤维层中添加氮化硅陶瓷粉，氧化铝纤维、石英纤维、高硅氧纤维添加氧化铝陶瓷粉，所述界面为碳化硅界面，所述基体材料为陶瓷。
上述混编纤维预制体增强的复合材料的制备方法采用以下顺序步骤：
步骤1，制备氮化硅陶瓷浆料，调整浆料Zeta电位至30mV，球磨形成稳定悬浮液；
步骤2，将碳纤维束、碳化硅纤维束、氧化铝纤维束、石英纤维束、高硅氧纤维束在陶瓷浆料中浸渍，然后从浆料中拉出，保持纤维束中陶瓷含量，80℃干燥12小时；
步骤3，将得到的各纤维浸渍料编织成三维薄壁结构，纤维在编织过程中采用织机边撑织造，其中碳纤维、碳化硅的经纱密度为6.0根/cm，在编织过程中加入氮化硅陶瓷粉，陶瓷粉末面密度为200g/m 2，氧化铝纤维、石英纤维、高硅氧纤维的经纱密度为8.0根/cm，在编织过程中加入氧化铝粉末，陶瓷粉末的面密度为180g/m 2；
步骤4，将得到的碳纤维、碳化硅纤维、氧化铝纤维、石英纤维、高硅氧纤维的三维薄壁结构依次按顺序嵌套；
步骤5，层与层之间通过树脂粘结方式形成三维整体结构预制体；
步骤6，对预制体在氩气气氛下700℃处理1小时；
步骤7，通过化学气相沉积制备碳化硅界面，以四氯硅烷和甲烷为源物质，沉积温度为500℃，沉积时间1小时；
步骤8，对于外层碳纤维，通过化学气相沉积制备碳基体，对于剩下的各层，采用硅溶胶浸渍制备二氧化硅基体，所选用的硅溶胶粒径为10～30nm，溶胶内加入玻璃空心微球或酚醛玻璃微球，微球含量<10％，85℃保温10小时脱水凝胶化，然后750℃保温1小时进行热处理，重复浸渍热解10个周期，得到陶瓷基复合材料。
制备的上述复合材料使用温度可达1400℃，材料的热膨胀系数小于4.5×10 -6/℃，热导率小于40W/m·K，耐烧蚀性能好，从防热层到隔热层内外层温差高于700℃，有效实现防热与隔热一体化。
上述仅为本发明的具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。

Claims (9)

  1. 一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，其特征在于，所述纤维预制体为由2～5种纤维编织而成的三维立体织物，所述纤维预制体中纤维体积分数为35％～65％，预制体中单种纤维的体积分数为5％～60％，预制体中纤维布或毡的层数为2～5层，各层厚度0.5～50mm，层与层之间通过针刺缝合、树脂粘结、加纱引纱和浅交弯联方式形成三维整体结构，纤维在编织过程中采用织机边撑织造；
    透波复合材料外层为石英纤维，内层为高硅氧纤维或玻璃纤维；
    吸波复合材料外层为氧化物纤维，中间层为碳化硅纤维，内层为碳纤维；
    高温结构材料外层为碳化硅纤维，内层为碳纤维；
    1400℃以下隔热复合材料外层为碳化硅纤维，中间层依次为碳纤维、氧化铝纤维，内层为玻璃纤维；
    1400℃以上防热复合材料外层为碳纤维，中间层依次为碳化硅纤维、氧化铝纤维、石英纤维，内层为高硅氧纤维；
    所述的纤维布或毡由1～3种纤维与0～3种陶瓷粉体组成，纤维布或毡中陶瓷粉体体积分数为0～30％，陶瓷粉体中粘结剂体积分数为0～5％，所述陶瓷粉体为碳化硅、碳化硼、碳化锆、碳化钽、碳化铪、氮化硅、氮化硼、氧化硅、氧化钙、氧化钇、氧化锆和氧化铝，所述界面为富勒烯、石墨烯、热解碳、碳化硅、氮化硼和氧化物界面，所述基体材料为树脂、轻合金、碳和陶瓷。
  2. 一种混编纤维预制体增强的复合材料，由纤维预制体、复合材料界面以及基体组成，其特征在于，所述纤维预制体为由2～5种纤维编织而成的三维立体织物，所述纤维预制体中纤维的体积分数为35％～65％，所述纤维预制体中单种纤维的体积分数为5％～60％；所述纤维预制体中的纤维以纤维布或纤维毡的形式存在；所述纤维预制体中的纤维布或纤维毡的层数为2～5层，各层的厚度为0.5～50mm，层与层之间通过针刺缝合、树脂粘结、加纱引纱或浅交弯联方式形成三维整体结构；所述纤维在编织成纤维布或纤维毡的过程中采用织机边撑织造；所述纤维预制体为透波复合 材料、吸波复合材料、高温结构材料、1400℃以下隔热复合材料或1400℃以上防热复合材料；
    所述透波复合材料的外层为石英纤维，内层为高硅氧纤维或玻璃纤维；
    所述吸波复合材料的外层为氧化物纤维，中间层为碳化硅纤维，内层为碳纤维；
    所述高温结构材料的外层为碳化硅纤维，内层为碳纤维；
    所述1400℃以下隔热复合材料的外层为碳化硅纤维，中间层依次为碳纤维和氧化铝纤维，内层为玻璃纤维；
    所述1400℃以上防热复合材料的外层为碳纤维，中间层依次为碳化硅纤维、氧化铝纤维和石英纤维，内层为高硅氧纤维；
    所述纤维布或纤维毡由1～3种纤维与0～3种陶瓷粉体组成，所述纤维布或纤维毡中陶瓷粉体的体积分数为0～30％，所述陶瓷粉体中的粘结剂的体积分数为0～5％，所述陶瓷粉体为碳化硅、碳化硼、碳化锆、碳化钽、碳化铪、氮化硅、氮化硼、氧化硅、氧化钙、氧化钇、氧化锆或氧化铝；
    所述复合材料界面为富勒烯、石墨烯、热解碳、碳化硅、氮化硼或氧化物界面；
    所述基体为树脂、轻合金、碳或陶瓷基体。
  3. 根据权利要求1或2所述的复合材料，其特征在于，所述陶瓷粉体的面密度为180～225g/m 2。
  4. 一种混编纤维预制体增强的复合材料的制备方法，其特征在于，包括以下顺序步骤：
    步骤1，制备陶瓷浆料，调整浆料Zeta电位，球磨形成稳定悬浮液；
    步骤2，将纤维束在陶瓷浆料中浸渍，然后从浆料中拉出，保持纤维束中陶瓷含量；
    步骤3，将纤维浸渍料缠绕、铺层、编织成二维布，或三维薄壁结构，纤维在编织过程中采用织机边撑织造；
    步骤4，将不同纤维种类的二维布叠加，或不同纤维的三维薄壁结构嵌套；
    步骤5，层与层之间通过针刺缝合、树脂粘结、加纱引纱和浅交弯联方式形成三维整体结构预制体；
    步骤6，对预制体真空或惰性气氛下300～1000℃处理；
    步骤7，对预制体制备界面；
    步骤8，通过先驱体浸渍热解制备陶瓷基体，得到陶瓷基复合材料；通过树脂传递模塑浸渍制备树脂基体，得到树脂基复合材料；通过真空压力浸渍制备合金基体，得到金属基复合材料。
  5. 一种混编纤维预制体增强的复合材料的制备方法，其特征在于，包括以下顺序步骤：
    步骤1，制备陶瓷浆料，调整浆料Zeta电位，球磨形成稳定悬浮液；
    步骤2，将纤维束在所述稳定悬浮液中浸渍，然后从稳定悬浮液中拉出，保持纤维束中陶瓷含量，得到纤维预浸料；
    步骤3，将所述纤维浸渍料缠绕、铺层、编织成二维布，或三维薄壁结构，纤维浸渍料在编织过程中采用织机边撑织造；
    步骤4，将不同纤维种类的二维布叠加，或不同纤维的三维薄壁结构嵌套；
    步骤5，层与层之间通过针刺缝合、树脂粘结、加纱引纱或浅交弯联方式形成三维整体结构预制体；
    步骤6，对所述三维整体结构预制体真空或惰性气氛下300～1000℃处理；
    步骤7，对预制体制备界面；
    步骤8，通过先驱体浸渍热解制备陶瓷基体，得到陶瓷基复合材料；
    或通过树脂传递模塑浸渍制备树脂基体，得到树脂基复合材料；
    或通过真空压力浸渍制备合金基体，得到金属基复合材料。
  6. 根据权利要求4或5所述的制备方法，其特征在于，所述步骤1的调整浆料Zeta电位为30～60mV。
  7. 根据权利要求4或5所述的制备方法，其特征在于，所述步骤6的处理的温度为700～100℃。
  8. 根据权利要求4或5所述的制备方法，其特征在于，所述步骤7的制备界面的方法为浸渍或气相沉积。
  9. 根据权利要求8所述的制备方法，其特征在于，所述步骤7中，当采用气相沉积制备复合材料界面热解碳时，所述气相沉积的参数包括：气源为丙烯，稀释气体为氮气，系统总压为10kPa，P N2/P C3H6为2：1，沉积温度为900℃，沉积时间为2小时。
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