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Method for preparation of ultra-high temperature ceramic matrix composite material containing boron nitride by in-situ reaction

A technology of ultra-high temperature ceramics and composite materials, applied in the field of ultra-high temperature ceramics, can solve the problems of limited application, easy to cause agglomeration, poor thermal shock resistance, etc., to achieve the effect of improving thermal shock resistance, avoiding agglomeration and low cost

Active Publication Date: 2017-06-06
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, document 2 (International Journal of Refractory Metals and Hard Materials, 2010, 28(2): 187-190) reported that even if prepared as a Zr(Hf)C-SiC composite material, its thermal shock resistance is poor, which means Greatly limit its application in the field of ultra-high temperature
Document 3 (Materials&Design, 2011,32(1):401-405) reported that the addition of BN can effectively increase the ZrB 2 -The thermal shock resistance of SiC composite materials, however, when adding BN directly, due to the special lamellar structure of BN, it is very easy to form a card house structure, which is easy to cause agglomeration

Method used

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  • Method for preparation of ultra-high temperature ceramic matrix composite material containing boron nitride by in-situ reaction
  • Method for preparation of ultra-high temperature ceramic matrix composite material containing boron nitride by in-situ reaction
  • Method for preparation of ultra-high temperature ceramic matrix composite material containing boron nitride by in-situ reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 46.04 grams of zirconium boride powder with a particle size of 1 micron, 42.93 grams of silicon nitride powder with a particle size of 10 microns and 11.03 grams of graphite powder with a particle size of 400 mesh were ball milled in a ball mill tank for 8 hours, dried and sieved. Then put it into a graphite mould, and cold-press to form it. The applied pressure is 20 MPa. After cold-pressing for 10 minutes, put it into a hot-press furnace for hot-press sintering. The heating rate is 20°C / min, heated to 2100°C and kept for 2 hours, and the pressure is gradually increased to 40MPa while the temperature is rising. The whole sintering process is carried out under nitrogen protection. The obtained reaction product is carried out XRD analysis (see figure 1 ), it can be found that the prepared composite material is mainly composed of zirconium nitride, silicon carbide, boron nitride and a small amount of zirconia, and the phases in the prepared composite material are uniform...

Embodiment 2

[0038]60.21 grams of hafnium boride powder with a particle size of 10 microns, 31.66 grams of silicon nitride powder with a particle size of 1 micron and 8.13 grams of graphite powder with a particle size of 200 mesh were ball milled in a ball mill jar for 24 hours, dried and sieved. Then put it into a graphite mould, and form it by cold pressing, the applied pressure is 10MPa, after cold pressing for 10 minutes, put it into a discharge plasma sintering furnace for sintering. The heating rate is 100°C / min, heated to 1800°C and kept for 10 minutes, and the pressure is gradually increased to 30MPa while the temperature is rising. The whole sintering process is carried out under nitrogen protection. In this example, the prepared composite material is mainly composed of hafnium nitride, silicon carbide, boron nitride and a small amount of hafnium oxide, hafnium nitride accounts for 57.2wt%, silicon carbide accounts for 26.4wt%, and boron nitride accounts for 14.6wt%. Hafnium oxid...

Embodiment 3

[0040] 52.97 grams of zirconium boride powder with a particle size of 10 microns, 32.97 grams of silicon nitride powder with a particle size of 5 microns and 14.1 grams of graphite powder with a particle size of 300 mesh were milled in a ball mill jar for 16 hours, dried and sieved. Then put it into a graphite mould, and cold-press to form it. The applied pressure is 20 MPa. After cold-pressing for 10 minutes, put it into a hot-press furnace for hot-press sintering. The heating rate is 20°C / min, heated to 2000°C and kept for 1 hour, and the pressure is gradually increased to 40MPa while the temperature is rising. The whole sintering process is carried out under nitrogen protection. The obtained reaction product is carried out XRD analysis (see image 3 ), it can be found that the prepared composite material is mainly composed of zirconium carbide, silicon carbide, boron nitride and a small amount of zirconium oxide, and each phase in the prepared composite material is uniform...

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Abstract

Belonging to the field of ultra-high temperature ceramics, the invention in particular relates to a method for preparation of an ultra-high temperature ceramic matrix composite material containing boron nitride by in-situ reaction. Raw materials include zirconium boride or hafnium boride powder, silicon nitride powder and graphite powder, and are mixed, and then the mixture is subjected to in-situ reaction hot pressing sintering or reaction sintering in a discharge plasma sintering furnace. Under a nitrogen atmosphere, the heating rate is 10-100DEG C / min, the sintering temperature is 1800DEG C-2100DEG C, the sintering time is 10min-2h, and the sintering pressure is 20MPa-40MPa. Therefore, a BN phase is uniformly introduced into an ultra-high temperature ceramic matrix through in-situ reaction so as to finally obtain a ZrN(HfN)-SiC-BN composite material or ZrC(HfC)-SiC-BN composite material. The composite material can be used a nozzle throat liner and jet vane of a solid rocket engine, and a nose cone, end, wing leading edge of ultra high speed aircrafts and other high temperature resistant structural components.

Description

technical field [0001] The invention belongs to the field of ultra-high-temperature ceramics, and specifically relates to a method for preparing an ultra-high-temperature ceramic-based composite material containing boron nitride by in-situ reaction. Background technique [0002] Ultra-high temperature ceramics generally refer to those transition metal borides, carbides and nitrides that can be used in a reaction atmosphere above 1800°C and have excellent high-temperature oxidation resistance and mechanical properties. Among these materials, ZrC (ZrN) and HfC (HfN) have high melting point, good chemical stability, high elastic modulus, excellent electrical conductivity, high hardness, good thermal conductivity, etc. It is suitable as a candidate material for high-temperature resistant structural components such as nozzle throat liners of solid rocket motors, gas rudders, and nose cones, ends, and wing leading edges of ultra-high-speed aircraft. [0003] Document 1 (Journal o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/583
Inventor 陈继新赵国瑞苗磊李美栓
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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