BNmf-Si3N4w/Si3N4复合材料的制备与性能

崔雪峰; 赵凯; 王玉生; 叶昉; 成来飞

doi:10.13801/j.cnki.fhclxb.20220630.005

BN_mf-Si₃N_4w/Si₃N₄复合材料的制备与性能

doi: 10.13801/j.cnki.fhclxb.20220630.005

西北工业大学　超高温结构复合材料重点实验室，西安 710072

基金项目: 国家自然科学基金(52072304)；国家科技重大专项(2017-VI-0007-0077)；高等学校学科创新引智计划(B08040)

详细信息

通讯作者:
叶昉，博士，副教授，博士生导师，研究方向为陶瓷基复合材料 E-mail: yefang511@nwpu.edu.cn

成来飞，博士，教授，博士生导师，研究方向为陶瓷基复合材料　E-mail: chenglf@nwpu.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2022-05-13
- 修回日期: 2022-06-06
- 录用日期: 2022-06-24
- 网络出版日期: 2022-07-04
- 刊出日期: 2022-08-22

Preparation and properties of BN_mf-Si₃N_4w/Si₃N₄composites

Science and Technology on Thermostructural Composite Materials Laboratory, Northwestern Polytechnical University, Xi′an 710072, China

摘要

摘要: 为制备一种介电性能和力学性能优异的高温透波材料，采用凝胶注模(GC)结合先驱体浸渍裂解(PIP)工艺制备了BN_mf-Si₃N_4w/Si₃N₄复合材料。研究了浸渍裂解次数及BN_mf含量对复合材料的力学性能与介电性能的影响。结果表明：(1) 随着PIP循环次数增加，复合材料的密度增大，气孔率降低，氮化硅基体逐渐形成三维网络结构包裹在复相微米增强体周围，复合材料力学性能提升；(2) 当BN_mf含量从4vol%增加到12vol%时，弯曲强度从175.5 MPa降低到139.3 MPa，断裂韧性从2.36 MPa·m^1/2增加到2.73 MPa·m^1/2，介电常数从3.62下降到3.25，介电损耗角正切从0.012下降到0.007；(3) BN_mf-Si₃N_4w/Si₃N₄复合材料的强韧化机制主要为裂纹分叉、裂纹偏转及BN_mf及Si₃N_4w的拔出，三种机制有效降低主裂纹对复合材料的损害。
- 凝胶注模 /
- 先驱体浸渍裂解 /
- 透波复合材料 /
- 介电性能 /
- 力学性能
Abstract: To prepare a high-temperature wave-transparent material with excellent dielectric and mechanical properties, the BN_mf-Si₃N_4w/Si₃N₄ composite material was prepared by gel-casting (GC) and precursor infiltration and pyrolysis (PIP) process. The effects of the cycles of PIP and the BN_mf content on the mechanical properties and dielectric properties of composite materials were studied. The results show that: (1) As the number of PIP cycles increases, the density of the composite material increases, the porosity decreases, and the mechanical properties improve. The silicon nitride matrix gradually forms a three-dimensional network structure wrapped around the multiphase micro-reinforcement; (2) When the content of BN_mf increases from 4vol% to 12vol%, the bending strength decreases from 175.5 MPa to 139.3 MPa, and the fracture toughness increases from 2.36 MPa·m^1/2 to 2.73 MPa·m^1/2, the dielectric constant decreases from 3.62 to 3.25, and the dielectric loss tangent decreases from 0.012 to 0.007; (3) The strengthening and toughening mechanisms of BN_mf-Si₃N_4w/Si₃N₄ composites are mainly crack bifurcation, crack deflection, and pull-out of BN_mf and Si₃N_4w. Three mechanisms effectively reduce the damage of the main crack to the composite.
- gel-casting /
- precursor infiltration pyrolysis /
- transparent composite material /
- mechanical properties /
- dielectric properties

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图 1 先驱体浸渍裂解(PIP)过程的增重率及其次数对BN_mf-Si₃N_4w/Si₃N₄复合材料开气孔率和密度的影响

Figure 1. Effect of mass gain rate of precursor infiltration pyrolysis (PIP) process and its number on the open porosity and density of BN_mf-Si₃N_4w/Si₃N₄ composites

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图 2 不同PIP循环次数的 BN_mf-Si₃N_4w/Si₃N₄复合材料断口的SEM图像：(a) SC41；(b) SC43；(c) SC45

Figure 2. SEM images of fracture morphology of BN_mf-Si₃N_4w/Si₃N₄ composites materials with different PIP cycles: (a) SC41; (b) SC43; (c) SC45

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图 3 不同PIP循环次数的BN_mf-Si₃N_4w/Si₃N₄复合材料的力学性能测试曲线：(a) 断裂韧性的载荷-位移曲线；(b) 三点弯的应力-位移曲线

Figure 3. Mechanical properties measurement curves of BN_mf-Si₃N_4w/Si₃N₄ composites with different PIP cycles: (a) Load-displacement curves of fracture toughness samples; (b) Stress-displacement curves of three-point bending samples

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图 4 不同PIP循环次数的BN_mf-Si₃N_4w/Si₃N₄复合材料的力学性能：(a) 断裂韧性；(b) 三点弯曲强度

Figure 4. Mechanical properties comparison of BN_mf-Si₃N_4w/Si₃N₄ composites with different PIP cycles: (a) Fracture toughness; (b) Three-point flexural strength

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图 5 不同增强体配比BN_mf-Si₃N_4w/Si₃N₄复合材料的XRD图谱

Figure 5. XRD patterns of BN_mf-Si₃N_4w/Si₃N₄ composites with different reinforcement ratios

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图 6 不同增强体配比BN_mf-Si₃N_4w/Si₃N₄复合材料抛光表面的SEM图像：(a) 4vol%BN_mf-36vol%Si₃N_4w；(b) 8vol%BN_mf-32vol%Si₃N_4w；(c) 12vol%BN_mf-28vol%Si₃N_4w

Figure 6. SEM images of polished surfaces of BN_mf-Si₃N_4w/Si₃N₄ composite materials with different reinforcement ratios: (a) 4vol%BN_mf-36vol%Si₃N_4w; (b) 8vol%BN_mf-32vol%Si₃N_4w; (c) 12vol%BN_mf-28vol%Si₃N_4w

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图 7 不同增强体配比BN_mf-Si₃N_4w/Si₃N₄复合材料的力学性能测试曲线：(a) 断裂韧性载荷-位移曲线；(b) 三点弯应力-位移曲线

Figure 7. Mechanical properties measurement curves of BN_mf-Si₃N_4w/Si₃N₄ composites with different reinforcement ratios: (a) Load-displacement curves of fracture toughness samples; (b) Stress-displacement curves of three-point bending samples

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图 8 不同增强体配比BN_mf-Si₃N_4w/Si₃N₄复合材料的力学性能：(a) 断裂韧性；(b) 三点弯曲强度

Figure 8. Mechanical properties of BN_mf-Si₃N_4w/Si₃N₄ composites with different reinforcement ratios: (a) Fracture toughness; (b) Three-point flexural strength

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图 9 BN_mf-Si₃N_4w/Si₃N₄复合材料的断口表面形貌：((a)~(c)) 裂纹在试样中扩展路径；(d) 裂纹横截面

Figure 9. SEM images of fracture surface morphologies of BN_mf-Si₃N_4w/Si₃N₄ composites: ((a)-(c)) Crack propagation; (d) Crack cross section

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图 10 不同增强体配比BN_mf-Si₃N_4w/Si₃N₄复合材料的介电性能

Figure 10. Dielectric properties of BN_mf-Si₃N_4w/Si₃N₄ composites with different reinforcement ratios

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表 1 BN_mf-Si₃N_4w预制体的命名

Table 1. Naming of BN_mf-Si₃N_4w preform

	BN_mf/vol%	PIP cycles
SC41	4	1
SC43	4	3
SC45	4	5
SC85	8	5
SC124	12	5
Note: PIP—Precursor infiltration pyrolysis.

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