Structural evolution of siloxane-epoxy crosslinked networks and their high-temperature electrical properties

YIN Kai; LI Jing; TENG Chenyuan; HU Yishuang; CHEN Xiangrong; ZHA Junwei

doi:10.7498/aps.74.20250654

Abstract

The ongoing trend toward high-power and miniaturized electronic devices has raised increasingly stringent requirements for the high-temperature electrical properties of epoxy encapsulating materials. In this study, epoxy-terminated phenyltrisiloxane (ETS) is used as a functional monomer to incorporate Si-O bonds into bisphenol-A epoxy resin through crosslinking reactions, thereby systematically investigating the influence and modulation effects of ETS on the structure and high-temperature electrical characteristics of epoxy composites. Gel content measurements indicate that as the concentration of ETS increases, the gel content of the epoxy resin composite decreases accordingly, suggesting that higher ETS content reduces the crosslinking density of the epoxy network. Experimental test results demonstrate that compared with pure epoxy resin, the composite with 2.5% ETS exhibits superior performance: the glass transition temperature increases to 129 ℃ with thermal decomposition temperature rising, while showing optimal high-temperature (70 ℃) electrical properties including significantly reduced conductivity, markedly suppressed space charge accumulation, deepened trap energy level (from 0.834 eV to 0.847 eV), reduced dielectric loss (0.005 at 50 Hz), and improved breakdown strength (74.2 kV/mm). Notably, as the ETS content increases, the electrical properties of epoxy composite follow a non-monotonic concentration dependence, initially enhancing then deteriorating, exhibiting evolutionary characteristics similar to those of nanoparticle-modified systems. Herein, a competitive mechanism between the epoxy network structure and intrinsic properties of ETS is proposed to explain this phenomenon: at low concentrations, the original C—C network dominates, where the intrinsic properties of ETS are constrained by the host matrix, leading to improved thermal stability. Simultaneously, the bandgap difference between ETS and DGEBA establishes charge barriers that can enhance insulation performance. However, at higher concentrations, the reduced crosslinking density and increased free volume caused by reactivity and structural mismatch between ETS and DGEBA ultimately lead to performance degradation. This study offers crucial theoretical insights into and produces the design strategies for developing high-performance siloxane-modified epoxy encapsulants.

Keywords:

Authors and contacts

1.
School of Information and Electrical Engineering, Hangzhou City University, Hangzhou 310015, China
2.
College of Electrical Engineering, Zhejiang University, Hangzhou 310027, China
3.
College of Information Engineering, Zhejiang University of Technology, Hangzhou 310023, China
4.
State Key Laboratory of Alternate Electrical Power System with Renewable Energy Sources, North China Electric Power University, Beijing 102206, China

Corresponding author: LI Jing, lijing@hzcu.edu.cn ; ZHA Junwei, zhajw@ncepu.edu.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 52207032) and the China Postdoctoral Science Foundation (Grant Nos. 2023M733031, 2024M751525).

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References

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Cited By

图 1 ETS单体的化学分子式

Figure 1. Molecular structure of ETS monomer.

DownLoad: Full-Size Img PowerPoint

图 2 两种环氧树脂单体的分子轨道能级分布　(a) DGEBA; (b) ETS

Figure 2. Energy level distribution of two types of epoxy monomers: (a) DGEBA; (b) ETS.

DownLoad: Full-Size Img PowerPoint

图 3 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP复合材料的凝胶含量

Figure 3. The gel content of Pure EP, 2.5% Si-EP, 5% Si-EP, and 10% Si-EP composites.

DownLoad: Full-Size Img PowerPoint

图 4 (a)—(d) Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP的SEM照片; (e), (f) 2.5% Si-EP表面C, O, Si元素分布及含量; (g), (h) 10% Si-EP表面C, O, Si元素分布及含量

Figure 4. (a)–(d) SEM of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples; (e), (f) distribution of C, O and Si elements and content on the surface of 2.5% Si-EP; (g), (h) distribution of C, O and Si elements and content on the surface of 10% Si-EP.

DownLoad: Full-Size Img PowerPoint

图 5 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP的XPS图谱以及Si-EP对应的Si 2p的精细图谱

Figure 5. XPS spectra of Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP samples, with insets showing high-resolution Si 2p spectra for the Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 6 Pure EP, 2.5% Si-EP, 5% Si-EP 和10% Si-EP的FTIR图谱

Figure 6. FTIR spectra of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 7 Pure EP, 2.5% Si-EP, 5% Si-EP 和10% Si-EP的DSC曲线

Figure 7. DSC curves of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 8 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP的热失重曲线

Figure 8. TGA curves of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 9 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP在不同场强下的电导率

Figure 9. Conductivity of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples at different applied electric fields.

DownLoad: Full-Size Img PowerPoint

图 10 (a) Pure EP, (b) 2.5% Si-EP, (c) 5% Si-EP和(d) 10% Si-EP在不同场强下空间电荷分布随时间的变化

Figure 10. Space charge distribution of (a) Pure EP, (b) 2.5% Si-EP, (c) 5% Si-EP and (d) 10% Si-EP samples at different applied electric fields.

DownLoad: Full-Size Img PowerPoint

图 11 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP平均电荷密度随时间的衰减

Figure 11. Decay of average charge density with time for Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 12 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP的陷阱能级

Figure 12. Trap energy levels of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 13 Pure EP, 2.5% Si-EP, 5% Si-EP 和10% Si-EP的宽频介电常数实部ε'

Figure 13. Broadband dielectric spectroscopy real part ε' of Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 14 (a) Pure EP, (b) 2.5% Si-EP, (c) 5% Si-EP和(d) 10% Si-EP的宽频介电虚部ε''弛豫响应分解

Figure 14. Broadband dielectric spectroscopy imaginary part ε'' of (a) Pure EP, (b) 2.5% Si-EP, (c) 5% Si-EP and (d) 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 15 Pure EP, 2.5% Si-EP, 5% Si-EP和10% Si-EP交流击穿场强的韦布尔分布

Figure 15. Weibull distribution of AC breakdown field strength for Pure EP, 2.5% Si-EP, 5% Si-EP and 10% Si-EP samples.

DownLoad: Full-Size Img PowerPoint

图 16 Pure EP, 2.5% Si-EP, 5% Si-EP, 10% Si-EP 环氧树脂交联网络随着ETS含量增大的演变示意图

Figure 16. Schematic diagram of the evolution of Pure EP, 2.5% Si-EP, 5% Si-EP, and 10% Si-EP cross-linked network with increasing ETS content.

DownLoad: Full-Size Img PowerPoint

DownLoad: Full-Size Img PowerPoint

表 1 Pure EP, Si-EP韦布尔概率分布参数

Table 1. Weibull distribution parameters for Pure EP and Si-EP samples.

Pure EP 2.5% Si-EP 5% Si-EP 10% Si-EP

β 68.3 74.2 72.6 67.2

σ 14.5 16.1 11.1 12.5

DownLoad: CSV

map

[1]	任俊文, 姜国庆, 陈志杰, 魏华超, 赵莉华, 贾申利 2024 73 027703 Google Scholar Ren J W, Jiang G Q, Chen Z J, Wei H C, Zhao L H, Jia S L 2024 Acta Phys. Sin. 73 027703 Google Scholar
[2]	Geng H R, Zhao L, Deng J, Chen J R, Fan Y H, Zhao Q Y, Gui H X, Liao J H, Zhao Y F, Qian Y X, Wang G Z 2025 Compos. Sci. Technol. 261 110993 Google Scholar
[3]	You Z Y, Weng L, Guan L Z, Zhang X R, Wu Z J, Chen H, Zhao W 2025 High Volt. 10 219 Google Scholar
[4]	Jiang C W, Hao C X, Zi C F, Li J, Liu W J, Bian Y M, Sun F Y, Xu Y Q, Yan Y X, Wang L Y, Su F Y, Tian Y Q 2025 Compos. Sci. Technol. 265 111135 Google Scholar
[5]	Xia G W, Xie J, Song Y Z, Duan Q J, Zhong Y Y, Xie Q 2025 Compos. Sci. Technol. 261 111019 Google Scholar
[6]	Yang X, Huang W J, Dong H, Zha J W 2025 Adv. Mater. 37 2500472 Google Scholar
[7]	Maes S, Badi N, Winne J M, Du Prez F E 2025 Nat. Rev. Chem. 9 144 Google Scholar
[8]	Yang K R, Dai J Y, Zhao W W, Wang S P, Liu X Q 2024 Compos. part B: Eng. 284 111728 Google Scholar
[9]	Zhou Y, LaChance A M, Wang Q, Gao Y F, Zhou J R, Huang B D, Shen K Y, Hou Z L, Lei T, Wang N Z, Zuo Z, Liu S, Dissado L A, Shao T, Liang X D, Cao Y, Sun L Y, Wu C, 2025 J. Mater. Chem. A 13 12926 Google Scholar
[10]	Wang Z Y, Sun X, Wang Y, Liu J D, Zhang C, Zhao Z B, Du X Y 2023 Ceram. Int. 49 2871 Google Scholar
[11]	黄家良, 高筱然, 郭亮, 宋思宇, 朱杰, 方志 2025 高电压技术 51 2476 Google Scholar Huang J L, Gao X R, Guo L, Song S Y, Zhu J, Fang Z 2025 High Volt. Eng. 51 2476 Google Scholar
[12]	邱甲云, 安秋凤, 史书源, 卢攀 2023 绝缘材料 56 1 Google Scholar Qiu J Y, An Q F, Shi S Y, Lu P 2023 Insul. Mater. 56 1 Google Scholar
[13]	Liu Y P, Li L, Liu H C, Zhang M J, Liu A J, Liu L, Tang L, Wang G L, Zhou S S 2020 Compos. Sci. Technol. 200 108418 Google Scholar
[14]	贺涛, 刘文凤, 冀运东 2024 热固性树脂 39 1 Google Scholar He T, Liu W F, Ji Y D 2024 Thermoset. Resin 39 1 Google Scholar
[15]	Jin B H, Jang J, Kang D J, Yoon S, Im H G 2022 Compos. Sci. Technol. 224 109456 Google Scholar
[16]	Wang C Z, Li S X, Yuan Y, Ji Y D, Cao D F 2024 Polymer 308 127368 Google Scholar
[17]	Zhang Y, Shi Y X, Jin C, Wu C, Dong H, Qu Z R, Song Y J 2025 React. Funct. Polym. 207 106114 Google Scholar
[18]	Singha S, Thomas M 2008 IEEE Trans. Dielect. Electr. Insul. 15 12 Google Scholar
[19]	Ma Y N, Zhao Z H, Zheng Z R, Li J W, Li M H, Hu J 2024 Matter 7 4046 Google Scholar
[20]	Gibbs G V, Wallace A F, Cox D F, Downs R T, Ross N L, Rosso K M 2009 Am. Mineral. 94 1085 Google Scholar
[21]	Rüchardt C, Beckhaus H 1980 Angew. Chem. Int. Ed. Engl. 19 429 Google Scholar
[22]	Sun B Z, Liang H L, Che D Y, Liu H P, Guo S 2019 RSC Adv. 9 9099 Google Scholar
[23]	Liu Z Y, Wang H, Chen Y Z, Kang G D, Hua L, Feng J D 2022 Polymers 14 512 Google Scholar
[24]	Yu M, Chen Z Y, Li J, Tan J H, Zhu X B 2023 Molecules 28 2826 Google Scholar
[25]	Weinhold F, West R 2011 Organometallics 30 5815 Google Scholar
[26]	Armstrong D A, Yu D, Rauk A 1996 Can. J. Chem. 74 1192 Google Scholar
[27]	Smith K L, Black K M 1984 J. Vac. Sci. Technol. A 2 744 Google Scholar
[28]	Berthomieu C, Hienerwadel R 2009 Photosynth. Res. 101 157 Google Scholar
[29]	Nabedryk E, Andrianambinintsoa S, Berger G, Leonhard M, Mäntele W, Breton J 1990 Biochim. Biophys. Acta–Bioenerg. 1016 49 Google Scholar
[30]	Yin K, Fan Q H, Li J, Rahman T U, Zhang T Y, Paramane A, Chen X R 2024 High Volt. 9 930 Google Scholar
[31]	Kim M T 1997 Thin Solid Films 311 157 Google Scholar
[32]	Oh T 2010 Phys. Status Solidi C 7 448 Google Scholar
[33]	Cao G, Yan Y, Zou X M, Zhu R S, Ouyang F Y 2018 Spectral Anal. Rev. 06 12 Google Scholar
[34]	Turchanin A, Käfer D, El-Desawy M, Wöll C, Witte G, Gölzhäuser A 2009 Langmuir 25 7342 Google Scholar
[35]	Dai X Z, Rumi A, Cavallini A, Bak C L, Hao J, Liao R J, Wang H 2024 IEEE Trans. Dielect. Electr. Insul. 31 2290 Google Scholar
[36]	Zhu Y W, Jiang Y H, Cao F H, Wang P J, Ke J X, Liu J, Nie Y J, Li G C, Wei Y H, Lu G H, Li S T 2025 J. Mater. Chem. C 13 11697 Google Scholar
[37]	Simmons J G, Tam M C 1973 Phys. Rev. B 7 3706 Google Scholar
[38]	Wang T Y, Mao J, Zhang B, Zhang G X, Dang Z M 2024 Nat. Rev. Electr. Eng. 1 516 Google Scholar
[39]	Wu C, Liang X D, Dissado L A, Chalashkanov N M, Dodd S J, Gao Y F, Xu S 2018 Compos. Sci. Technol. 163 56 Google Scholar
[40]	Fu J Y 2014 Philos. Mag. 94 1788 Google Scholar
[41]	Wu K N, Sui H R, Ren Y R, Yang K, Zhao P, Ouyang B H, Li H, Zhang X, Ran L, Li J Y 2025 IEEE Trans. Dielect. Electr. Insul. 32 815 Google Scholar
[42]	Wang Q L, Chen X R, Li J Y, Paramane A, Huang X F, Ren N 2024 IEEE Trans. Dielect. Electr. Insul. 31 1823 Google Scholar
[43]	高铭泽, 张沛红 2016 65 247802 Google Scholar Gao M Z, Zhang P H 2016 Acta Phys. Sin. 65 247802 Google Scholar
[44]	Grabowsky S, Beckmann J, Luger P 2012 Aust. J. Chem. 65 785 Google Scholar
[45]	Chen J, Zhou Y, Huang X Y, Yu C Y, Han D L, Wang A, Zhu Y K, Shi K M, Kang Q, Li P L, Jiang P K, Qian X S, Bao H, Li S T, Wu G N, Zhu X Y, Wang Q 2023 Nature 615 62 Google Scholar

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Vol. 74, Issue 19 - 2025-10-05

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