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Preparation method of ablation-resistant quartz fiber reinforced silicon oxide based composite material

A technology of quartz fibers and composite materials, applied in the field of composite materials, can solve the problems of weakening the strength of composite materials, and achieve the effects of improving strength retention, improving high temperature resistance, and strong operability

Active Publication Date: 2019-01-22
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, in the process of increasing the density, it is easy to greatly weaken the strength of the composite material. How to maintain the strength of the composite material at a high level while increasing the density is also a problem that needs to be solved.

Method used

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  • Preparation method of ablation-resistant quartz fiber reinforced silicon oxide based composite material

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preparation example Construction

[0028] A method for preparing an ablation-resistant quartz fiber reinforced silica-based composite material, comprising the steps of:

[0029] (1) Use Al element doped quartz fiber to weave high-density orthogonal three-way fabric preform, and use cyclic vacuum impregnation high-purity silica sol process for the fabric preform to make the material density reach or exceed 1.76g / cm 3 After that, SiO was impregnated by vacuum pressure method 2 Ethyl orthosilicate with content ≥ 40%;

[0030] (2) Carry out acid steaming treatment to the material obtained in the above steps, so that the tetraethyl orthosilicate in the material is hydrolyzed in situ, and subsequently, the material is subjected to drying and dehydration treatment;

[0031] (3) After repeating the steps of impregnating tetraethyl orthosilicate, acid steaming, and drying and dehydrating for 1 to 3 times, until the density of the material no longer increases significantly, the final material is obtained after vacuum he...

Embodiment 1

[0048] The volume density is 1.28g / cm by weaving high-purity quartz fiber with Al doping amount of 500ppm 3 , an orthogonal three-way fabric preform with a size of 100×100×30mm; immerse the fabric preform as a whole in a high-purity silica sol with a purity ≥ 99.9% in an impregnation tank, then seal the impregnation tank and evacuate to a vacuum degree of - 0.1MPa, keep for 60min after reaching the target vacuum degree, then return to normal pressure, take out the impregnated fabric preform, dry at 80°C for 500min, then raise the temperature to 200°C for 60min. After repeating the above whole impregnation and drying steps 5 times, the material density reached 1.76g / cm 3 . Carry out heat treatment on the material, the heat treatment temperature is 600°C, and the holding time is 180min; the material obtained in the above steps is immersed in the SiO2 dipping tank as a whole 2 In tetraethyl orthosilicate with a content ≥ 40%, then seal the impregnation tank and evacuate to a va...

Embodiment 2

[0050] The bulk density is 1.32g / cm by weaving high-purity quartz fiber with Al doping amount of 300ppm 3 , an orthogonal three-way fabric preform with a size of 300×300×28mm; immerse the fabric preform as a whole in a high-purity silica sol with a purity ≥ 99.9% in an impregnation tank, then seal the impregnation tank and evacuate to a vacuum degree of - 0.06MPa, keep it for 120min after reaching the target vacuum degree, then return to normal pressure, take out the impregnated fabric preform, dry at 90°C for 300min, then raise the temperature to 120°C for 180min. After repeating the entire impregnation and drying steps above 9 times, the material density reached 1.80 g / cm 3 . Carry out heat treatment on the material, the heat treatment temperature is 800°C, and the holding time is 60min; the material obtained in the above steps is immersed in the SiO2 dipping tank as a whole 2 In tetraethyl orthosilicate with a content ≥ 40%, then seal the impregnation tank and evacuate to...

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Abstract

The invention relates to a preparation method of an ablation-resistant quartz fiber reinforced silicon oxide based composite material. According to the preparation method, Al doped high purity quartzfiber with higher heat resistant grade is adopted to replace common quartz fiber in weaving of a fabric prefab; ethyl orthosilicate dipping and acid steaming are adopted to increase composite densityto be higher than 2.0g / cm<3>; and at last at 850 to 1050 DEG C, long term of vacuum heat processing is carried out. The ethyl orthosilicate dipping and acid steaming are adopted to solve a problem inthe prior art that further increasing of composite material density is impossible to realize through conventional circulation dipping of silica sol. The preparation method is capable of increasing ablation resistance of the composite material at typical ablation states at a temperature higher than 2000 DEG C by more than 50%, and at the same time, the tensile strength is maintained to be higher than 30MPa. The preparation method is high in operationality, and is suitable to be used in the field of quartz fiber reinforced silicon oxide based composite material engineering preparation.

Description

technical field [0001] The invention relates to a preparation method of an ablation-resistant quartz fiber reinforced silica-based composite material, which belongs to the technical field of composite materials. Background technique [0002] Quartz fiber reinforced silica-based composite material is a composite material that integrates wave transmission, load bearing and heat insulation. Ablation resistance in extreme thermal environments is one of its important indicators, and for a specific material system, density is one of the most critical factors determining its ablation resistance, the higher the density, the more ablation resistance. [0003] At present, the mature preparation process of this material is the cyclic impregnation process of high-purity silica sol. The high-purity quartz fiber fabric is impregnated with silica sol and dried, and this cycle is repeated several times. After heat treatment, quartz fiber reinforced silica is finally obtained. base composit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/66C04B35/80C04B35/14
CPCC04B35/803C04B35/14C04B35/66C04B2235/5216C04B2235/656C04B2235/6567C04B2235/6581C04B2235/77C04B2235/96
Inventor 周军张大海张敬义
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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