Dielectric properties measurements on silicon nitride fiber based on high-Q cavity method
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摘要: 氮化硅纤维具有优异的耐高温性能和透波能力，是理想的高温透波增强材料。本文对高Q腔法测试陶瓷纤维介电性能的样品制备和测试方法进行了研究和优化。研究发现，介电测试试样中纤维含量应不低于20wt%，含量过低易导致计算所得的纤维介电常数偏低；同时短切纤维的长度主要影响介电测试数据的离散性，由长度不大于1.0 mm的短纤维所制试样质量高，介电测试结果稳定性更佳。对比讨论了Lichtenecker、Bruggeman和Looyenga三种介电混合模型的适用性，最终基于Lichtenecker介电常数对数混合法则计算得到石英纤维的相对介电常数与文献报道数据较一致。分析表明，氮化硅纤维在10 GHz频率下的相对介电常数为4.4，损耗角正切值为0.0005，是优异的低介电高透波材料。同时，表面上浆剂通过改变纤维表面极性特征，对氮化硅纤维介电性能尤其介电损耗产生显著影响。Abstract: The silicon nitride fiber has excellent high temperature resistance and wave transmission capability, which is an ideal reinforcement using for high-temperature wave-transparent composites. In this paper, preparation and test methods for the dielectric properties of ceramic fibers tested by high-Q cavity method were studied and optimized for continuous ceramic fibers. The study shows that the fiber content in the dielectric test sample should be no less than 20wt%, and less fiber content tended to result in a relatively smaller value of the fiber dielectric constant. Meanwhile, the length of chopped fiber has effect on the repeatability of the fiber dielectric properties. The samples made by the chopped fiber with the length no more than 1.0 mm are of high quality and the resulted fiber dielectric data are more reliable. In terms of data processing, the applicability of three dielectric mixing models of Lichtenecker, Bruggeman and Looyenga was discussed in comparison. Finally, the permittivity of quartz fibers was calculated based on Lichtenecker dielectric constant logarithmic mixing rule, which was consistent with the reported data. It has been found that the silicon nitride fiber has a permittivity of 4.4 and a loss tangent of 0.0005 at 10 GHz, demonstrating excellent low dielectric. Furthermore, it shows that the surface sizing agent has a significant effect on the dielectric properties particularly the loss tangent of the silicon nitride fiber, which is associated with its surface polarity characteristics of the silicon nitride fiber.
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图 1 不同方式去剂前后氮化硅纤维表面的SEM图像
SIN-B—Bare fibers; SIN-S—As-received fibers; SIN-A—Fibers removed sizing agent with acetone; SIN-H—Fibers removed sizing agent with water
Figure 1. SEM images of surface of silicon nitride fibers before and after sizing removal in different ways (((a), (b)) SIN-B; ((c), (d)) SIN-S; ((e), (f)) SIN-A; ((g), (h)) SIN-H)
图 2 不同方法制备的氮化硅纤维/石蜡复合材料介电测试试样
Figure 2. Dielectric test samples of silicon nitride fiber/paraffin wax composites prepared by different methods
图 3 不同纤维含量的氮化硅纤维/石蜡复合材料依据三种混合模型估算所得氮化硅纤维的相对介电常数
Figure 3. Permittivities of silicon nitride fiber evaluated by three dielectric mixture models according to silicon nitride fiber/paraffin wax composites with different fiber contents
图 4 不同切割长度的氮化硅纤维/石蜡复合材料的相对介电常数
Figure 4. Relative permittivity of silicon nitride fiber/paraffin wax composites with different chopped lengths of silicon nitride fiber
图 5 不同切割长度的氮化硅纤维/石蜡复合材料的照片
Figure 5. Photographs of silicon nitride fiber/paraffin wax composites with different chopped lengths of silicon nitride fiber
图 6 同一氮化硅纤维/石蜡复合材料不同时间相对介电常数测试结果
Figure 6. Permitvities of silicon nitride fiber/paraffin wax composites sample obtained at different times
图 7 高Q腔法测试得到的石英纤维的相对介电常数
Figure 7. Permittivities of quartz fiber based on high-Q cavity method
图 8 不同方式去剂的氮化硅纤维的相对介电常数及损耗角正切
Figure 8. Permittivities and dielectric loss tangent of silicon nitride fibers after sizing removal by different methods
表 1 表面能测试试剂相关参数
Table 1. Parameters of surface energy test reagent
Reagent Surface energy/(mJ·m–2) $\gamma _{\rm{L} }^{}$ $\gamma _{\rm{L}}^{\rm{d}} $ $\gamma _{\rm{L}}^{\rm{p}} $ H2O 72.8 21.8 51.0 Formamide 58.2 39.5 18.7 Methylene iodide 50.8 48.5 2.3 Notes：${\gamma _{\rm{L} }^{} }$,$\gamma _{\rm{L}}^{\rm{d}} $, $\gamma _{\rm{L}}^{\rm{p}} $—Solid-liquid surface tension, dispersion and polarity property, respectively. 
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表 2 不同方法制备的氮化硅纤维/石蜡复合材料及反演的氮化硅纤维的介电性能
Table 2. Dielectric properties of silicon nitride fiber/paraffin wax composites and silicon nitride fiber prepared by different methods
Type Frequency/
MHzPermittivity by test Permittivity of fiber calculated by Lichtenecker formula ε1 ε2 Average ε1 ε2 Difference Average UB 7 382 2.33 2.34 2.34 2.33 3.23 0.90 2.74 8 173 2.33 2.35 2.34 2.33 4.47 2.14 3.23 9 335 2.33 2.35 2.34 2.33 4.47 2.14 3.23 10 736 2.33 2.35 2.34 2.33 4.47 2.14 3.23 12 283 2.33 2.35 2.34 2.33 4.47 2.14 3.23 13 914 2.34 2.35 2.35 3.23 4.47 1.24 3.80 15 607 2.33 2.35 2.34 2.33 4.47 2.14 3.23 17 348 2.33 2.34 2.34 2.33 3.23 0.90 2.74 FMB 7 382 2.49 2.49 2.49 4.75 4.75 0 4.75 8 173 2.49 2.50 2.50 4.75 4.95 0.20 4.85 9 334 2.49 2.50 2.50 4.75 4.95 0.20 4.85 10 733 2.49 2.49 2.49 4.75 4.75 0 4.75 12 277 2.47 2.49 2.48 4.38 4.75 0.37 4.56 13 905 2.47 2.49 2.48 4.38 4.75 0.37 4.56 15 592 2.47 2.48 2.48 4.38 4.56 0.18 4.47 17 331 2.46 2.48 2.47 4.20 4.56 0.36 4.38 Notes：ε1, ε2—Permittivity of the front and back of the samples or fibers; Difference and average are the differences and averages of ε1 and ε2.
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表 3 氮化硅纤维上浆剂薄膜丙酮处理前后的表面能及极性/色散比
Table 3. Surface energy and ratio of polarity to dispersion of silicon nitride fibers’ sizing film before and after treated by acetone
Sample Surface energy $\gamma _{\rm{S} }^{}$/
(mJ·m–2)$\gamma_{\rm{S} }^{\rm{p} }$/
(mJ·m–2)$\gamma_{\rm{S} }^{\rm{d} }$/
(mJ·m–2)$\gamma_{\rm{S} }^{\rm{p} }$/$\gamma_{\rm{S} }^{\rm{d} }$ Sizing film 63.6 22.3 41.4 0.54 Acetone treated sizing film 67.2 34.1 33.1 1.03 Notes:${\gamma _{\rm{S} }^{} }$,$\gamma _{\rm{S}}^{\rm{d}} $, $\gamma _{\rm{S}}^{\rm{p}} $—Solid surface energy, dispersion and polarity property, respectively.
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