硼酸辅助构筑多酸/乳糖衍生缺陷多孔碳及其高效微波吸收

doi:10.15541/jim20260113

无机材料学报 ›› 2026, Vol. 41 ›› Issue (10): 1470-1480.DOI: 10.15541/jim20260113

硼酸辅助构筑多酸/乳糖衍生缺陷多孔碳及其高效微波吸收

石金钊¹(), 朱美玲¹, 郑琦¹^,²(), 王连军¹^,²(), 江莞¹

¹ 东华大学材料科学与工程学院, 先进纤维材料全国重点实验室, 上海 201620
² 东华大学先进玻璃制造技术教育部工程研究中心, 上海 201620

收稿日期:2026-03-13 修回日期:2026-04-12 出版日期:2026-10-20 网络出版日期:2026-05-08
通讯作者: 郑琦, 教授. E-mail: qi.zheng@dhu.edu.cn;
王连军, 教授. E-mail: wanglj@dhu.edu.cn
作者简介:石金钊(1999-), 男, 硕士研究生. E-mail: 2230364@mail.dhu.edu.cn
基金资助:
国家自然科学基金(52372040);国家自然科学基金(52572068)

Boric Acid-assisted Construction of Polyoxometalate/Lactose-derived Defective Porous Carbon for Highly Efficient Microwave Absorption

SHI Jinzhao¹(), ZHU Meiling¹, ZHENG Qi¹^,²(), WANG Lianjun¹^,²(), JIANG Wan¹

¹ State Key Laboratory of Advanced Fiber Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China
² Engineering Research Center of Advanced Glass Manufacturing Technology, Ministry of Education, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China

Received:2026-03-13 Revised:2026-04-12 Published:2026-10-20 Online:2026-05-08
Contact: ZHENG Qi, professor. E-mail: qi.zheng@dhu.edu.cn;
WANG Lianjun, professor. E-mail: wanglj@dhu.edu.cn
About author:SHI Jinzhao (1999-), male, Master candidate. E-mail: 2230364@mail.dhu.edu.cn
Supported by:
National Natural Science Foundation of China(52372040);National Natural Science Foundation of China(52572068)

摘要/Abstract

摘要：

开发兼具轻质、宽频与强吸收特性的微波吸收材料, 对于复杂电磁环境下的防护具有重要意义。本研究以天然乳糖为碳源, 设计了一系列组分可调的多酸衍生金属钨酸盐与钨氧化物及多孔碳复合材料(WX@LC, X=Mn, Fe, Co)。实验采用乳糖为碳源, 以缺位多酸(SiW₉)配位组装的过渡金属取代多酸(W₁₈X)作为无机前驱体, 将其与硼酸充分混合辅助造孔后, 通过一步空气热解策略成功合成了该复合材料。微观结构分析表明, 纯碳基底仅具备由硼酸辅助造孔促成的高度互连的三维多孔导电网络; 引入多酸前驱体后, WX@LC复合材料内部精准构筑了高浓度氧空位以及晶体与无定形碳的异质界面。此外, 在Mn掺杂的WM@LC样品中观测到了MnWO₄与WO_2.83的双相异质界面。这种WM@LC独有的多重异质结构网络诱发了极强的界面极化, 同时保持了适度电导损耗, 有效优化了阻抗匹配。吸波性能测试结果表明, WM@LC展现出最优的吸波性能, 在15%(质量分数)填充量下, 匹配厚度为4.11 mm时, 最低反射损耗(RL_min)达-73.13 dB; 匹配厚度为2.18 mm时, 最大有效吸收带宽(EAB_max)达6.64 GHz, 完全覆盖Ku波段。本研究为碳基吸波材料的微观结构设计提供了一种有效途径, 并为多酸衍生物在电磁防护领域的应用提供了可靠参考。

关键词: 多金属氧酸盐, 微波吸收, 生物衍生碳, 异质界面

Abstract:

Developing lightweight, broadband, and highly efficient microwave absorption materials is of great significance for electromagnetic protection in complex environments. In this study, a series of composition-tunable composites (WX@LC, X = Mn, Fe, Co) consisting of polyoxometalate (POM)-derived metal tungstate, tungsten oxide, and porous carbon were designed. Using lactose as the carbon source and transition metal-substituted POMs as inorganic precursors, the composites were successfully synthesized via a facile one-step air pyrolysis strategy with boric acid as a pore-forming agent. Microstructural analysis reveals that introducing the POM precursor precisely constructs a high concentration of oxygen vacancies and rich heterogeneous interfaces within the highly interconnected 3D porous carbon network. Furthermore, a dual-phase heterogeneous interface between MnWO₄ and WO_2.83 is exclusively observed in the Mn-doped WM@LC sample. This unique multiple heterogeneous structure induces strong interfacial polarization while maintaining moderate conduction loss, which effectively optimizes impedance matching. Electromagnetic measurements demonstrate that WM@LC exhibits optimal microwave absorption performance. At a low filler loading of 15% (in mass), it achieves a minimum reflection loss (RL_min) of -73.13 dB at a thickness of 4.11 mm, and a maximum effective absorption bandwidth (EAB_max) of 6.64 GHz at 2.18 mm, fully covering the Ku band. This work offers an effective pathway for designing the microstructure of carbon-based microwave absorbers and provides a reliable reference for applying POM derivatives in electromagnetic protection.

Key words: polyoxometalate, microwave absorption, bio-derived carbon, heterointerface

中图分类号:

TB34

石金钊, 朱美玲, 郑琦, 王连军, 江莞. 硼酸辅助构筑多酸/乳糖衍生缺陷多孔碳及其高效微波吸收[J]. 无机材料学报, 2026, 41(10): 1470-1480.

SHI Jinzhao, ZHU Meiling, ZHENG Qi, WANG Lianjun, JIANG Wan. Boric Acid-assisted Construction of Polyoxometalate/Lactose-derived Defective Porous Carbon for Highly Efficient Microwave Absorption[J]. Journal of Inorganic Materials, 2026, 41(10): 1470-1480.

图/表 15

图1 硼酸模板辅助热解法制备WX@LC复合材料的实验流程示意图

Fig. 1 Schematic diagram of the experimental procedure for preparing WX@LC composites by boric acid template-assisted pyrolysis

图2 WX@LC复合材料的TEM照片及其元素分布

Fig. 2 TEM images and corresponding elemental distributions of WX@LC composites (a, d, g) TEM images; (b, e1, e2, h1, h2) HRTEM images; (c, f, i) STEM images and corresponding EDS elemental mappings; (a-c) WM@LC; (d, e1, e2, f) WF@LC; (g, h1, h2, i) WC@LC

图3 样品的物相结构与表面化学成分表征

Fig. 3 Characterization of phase structure and surface chemical composition of the samples (a) XRD patterns; (b) Raman spectra; (c) XPS full spectra; (d-f) High-resolution XPS spectra of (d) C1s, (e) O1s and (f) W4f, which reveal the coexistence of oxygen vacancies and multiple valence states of tungsten. Colorful figures are available on website

图4 样品的微波吸收性能表征

Fig. 4 Microwave absorption performance characterization of the samples (a1-d1) Three-dimensional reflection loss plots; (a2-d2) Corresponding two-dimensional RL contour plots; (a3-d3) Impedance matching Smith chart. Colorful figures are available on website

图5 样品的电磁参数、介电损耗机制及吸波性能对比

Fig. 5 Comparison of electromagnetic parameters, dielectric loss mechanisms, and microwave absorption performance of the samples (a) Real part of complex permittivity (ε'); (b) Imaginary part of complex permittivity (ε''); (c) Dielectric loss tangent (tanδE); (d) Attenuation constant (α); (e) Conduction loss (εc''); (f) Polarization relaxation (εp''); (g-j) Cole-Cole curves; (k) Conductivity histogram; (l) Comparison of microwave absorption performance. Colorful figures are available on website

图6 WM@LC的吸波机理图

Fig. 6 Microwave mechanism of WM@LC

图S1 W18Mn、W18Fe和W18Co样品的实验与模拟XRD谱图对比

Fig. S1 Comparison of experimental and simulated XRD patterns for W18Mn, W18Fe, and W18Co samples

图S2 样品的SEM照片

Fig. S2 SEM images of the samples (a1-d1) Low-magnification SEM images of LC, WM@LC, WF@LC and WC@LC; (a2-d2) High-magnification SEM images of the corresponding samples

图S3 LC的TEM照片及C元素分布

Fig. S3 TEM image and C elemental distribution of LC

图S4 样品的孔隙结构表征

Fig. S4 Pore structure characterization of the samples (a1-d1) Nitrogen adsorption-desorption isotherms; (a2-d2) Pore size distribution curves

图S5 SiW12@LC样品的XRD谱图

Fig. S5 XRD pattern of SiW12@LC sample

图S6 样品的XPS高分辨谱图

Fig. S6 High-resolution XPS spectra of the samples (a) Mn2p; (b) Fe2p; (c) Co2p

图S7 WX@LC的EPR图谱

Fig. S7 EPR spectra of WX@LC

图S8 样品的复磁导率和磁损耗特性

Fig. S8 Complex permeability and magnetic loss characteristics for samples (a) Real part of complex permeability (μ'), (b) Imaginary part of complex permeability (μ''), (c) Magnetic loss tangent (tanδM)

表S1 WM@LC与近期生物衍生碳/先进碳基吸波材料综合性能对比表

Table S1 Comparison of the overall performance of WM@LC with recent bio-derived carbon/advanced carbon-based microwave absorbing materials

Sample	RL_min/dB	Thickness/mm	EAB_max/GHz	Thickness/mm	Loading/% (in mass)	Ref.
FCCMT	-39.08	1.9	6.85	1.9	30	[55]
CoNi-MOF-Se-500	-51.1	1.8	4	1.8	25	[52]
C/Fe₃O₄	-40.1	2	5.12	2	50	[57]
WCA/BiCo@NC	-50.92	1.4	4.88	1.4	40	[53]
HCMs-900	-57.5	2.5	5.76	1.8	15	[22]
NiS/Co₃S₄/NiCoQCNTs/NC	-75.9	2.6	4.8	2.6	30	[56]
FCM	-52.59	1.92	6.04	2.2	30	[54]
NiO/NiFe₂O₄/Ni/Ni₃Fe@BC	-67.44	2.773	6.7	1.754	25	[51]
Fe-BBCN/Ti₃C₂T_x	-46.8	2	4.2	1.5	30	[58]
HPC-650	-49.96	1.5	6.46	2.4	30	[59]
PNBC/CoFe₂/CoFe₂O₄	-52.21	1.44	4.32	1.44	30	[60]
WM@LC	-73.13	4.11	6.64	2.18	15	This work

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硼酸辅助构筑多酸/乳糖衍生缺陷多孔碳及其高效微波吸收

Boric Acid-assisted Construction of Polyoxometalate/Lactose-derived Defective Porous Carbon for Highly Efficient Microwave Absorption

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