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摘要: 采用纯纳米AlN粉和掺杂质量分数3%Y2O3的纳米AlN粉为原料，经放电等离子烧结工艺制备AlN陶瓷，研究了两类AlN陶瓷的相对密度、微观组织、力学性能和导热性能。结果表明：纯纳米AlN粉和掺杂Y2O3纳米AlN粉在40～60 MPa下，经1500 ℃放电等离子烧结5～60 min，均可获得相对密度＞99%的AlN陶瓷。当烧结压力为50 MPa时，获得的AlN陶瓷晶粒尺寸最小，分别为176 nm和190 nm，细化晶粒明显提高了AlN陶瓷硬度和抗弯强度。当烧结时间从5 min延长至60 min时，两种AlN陶瓷晶粒尺寸分别增大至1.71 μm和1.73 μm。晶粒长大导致AlN陶瓷硬度和抗弯强度下降，但提升了导热性能。通过对比发现，相同放电等离子烧结工艺下添加烧结助剂Y2O3能够有效提升AlN陶瓷的综合性能。Abstract: AlN ceramics were prepared by spark plasma sintering (SPS) using the pure nano-AlN powders and the nano-AlN powders doped by 3% Y2O3 (mass fraction) as the raw materials. The relative density, microstructure, mechanical properties, and thermal conductivity of two types of AlN ceramics were studied. The results show that, both the pure nano-AlN powders and the nano-AlN powders doped by Y2O3 can obtain the AlN ceramics with the relative density above 99% prepared by SPS at 1500 ℃ for 5~60 min under 40~60 MPa. When the sintering pressure is 50 MPa, the average grain size of the AlN ceramics is the smallest, which is 176 nm and 190 nm, respectively. The hardness and bending strength of the AlN ceramics are obviously improved by the grain refinement. When the sintering time is extended from 5 min to 60 min, the grain size of the AlN ceramics is increased to 1.71 μm and 1.73 μm, respectively. The grain growth leads to the decrease of hardness and bending strength of the AlN ceramics, but improves the thermal conductivity. It is found that the addition of Y2O3 sintering agent can effectively improve the comprehensive properties of the AlN ceramics under the same SPS sintering process.
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Key words:
- AlN ceramics /
- spark plasma sintering /
- grain refinement /
- Y2O3
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图 2 不同烧结时间AY0和AY3试样断口的场发射扫描电子显微镜背散射形貌：（a）AY0，5 min；（b）AY0，30 min；（c）AY0，60 min；（d）AY3，5 min；（e）AY3，30 min；（f）AY3；60 min
Figure 2. FESEM back scatter images of the AY0 and AY3 fracture microstructures with the different sintering times: (a) AY0, 5 min; (b) AY0, 30 min; (c) AY0, 60 min; (d) AY3, 5 min; (e) AY3, 30 min; (f) AY3, 60 min
图 3 AY0和AY3试样硬度和抗弯强度与烧结时间关系：（a）维氏硬度；（b）抗弯强度
Figure 3. Hardness and bending strength of AY0 and AY3 with the different sintering times: (a) Vickers hardness; (b) bending strength
图 4 不同烧结压力下AY0和AY3试样断口场发射扫描电子显微镜背散射形貌：（a）AY0，40 MPa；（b）AY0，50 MPa；（c）AY0，60 MPa；（d）AY3，40 MPa；（e）AY3，50 MPa；（f）AY3；60 MPa
Figure 4. FESEM back scatter images of the AY0 and AY3 fracture microstructures with the different pressures: (a) AY0, 40 MPa; (b) AY0, 50 MPa; (c) AY0, 60 MPa; (d) AY3, 40 MPa; (e) AY3, 50 MPa; (f) AY3, 60 MPa
图 5 AY0和AY3试样力学性能随压力变化关系：（a）维氏硬度；（b）抗弯强度
Figure 5. Mechanical properties of AY0 and AY3 under the different pressures: (a) Vickers hardness; (b) bending strength
图 6 AY0和AY3试样晶粒尺寸与抗弯强度关系
Figure 6. Relationship between the grain size and bending strength of the AY0 and AY3 samples
图 7 AY0和AY3试样热导率（a）和物相组成（b）随烧结时间变化
Figure 7. Thermal conductivity (a) and phases composition (b) of AY0 and AY3 with the different sintering times
表 1 不同烧结时间放电等离子烧结试样的相对密度和平均晶粒尺寸
Table 1. Relative densities and the average grain sizes of the SPS samples for the different sintering times
样品 相对密度 / % 晶粒尺寸 / nm 5 min 30 min 60 min 5 min 30 min 60 min AY0 99.25 99.46 99.33 283 332 1710 AY3 99.12 99.39 99.07 767 1670 1730 
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表 2 不同烧结压力下试样的平均晶粒尺寸和相对密度
Table 2. Average grain sizes and the relative densities of the SPS samples under the different pressures
样品 相对密度 / % 晶粒尺寸 / nm 40 MPa 50 MPa 60 MPa 40 MPa 50 MPa 60 MPa AY0 99.06 99.56 99.48 283 176 574 AY3 99.27 99.44 99.52 513 190 353
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