超低介电常数LiBxAl1-xSi2O6微波介质陶瓷的低温烧结

doi:10.15541/jim20240494

无机材料学报 ›› 2025, Vol. 40 ›› Issue (5): 536-544.DOI: 10.15541/jim20240494

超低介电常数LiB_xAl_1-_xSi₂O₆微波介质陶瓷的低温烧结

熊思宇¹(), 莫尘¹, 朱肖伟¹, 朱国斌¹, 陈德钦¹, 刘来君¹, 施晓东², 李纯纯¹()

1.桂林理工大学材料科学与工程学院, 桂林 541004
2.桂林理工大学物理与电子信息工程学院, 桂林 541004

收稿日期:2024-11-27 修回日期:2024-12-19 出版日期:2025-05-20 网络出版日期:2025-01-09
通讯作者: 李纯纯, 副研究员. E-mail: lichunchun2003@126.com
作者简介:熊思宇(2000-), 女, 硕士研究生. E-mail: xiongsiyu0927@163.com
基金资助:
国家自然科学基金(62061011)

Low-temperature Sintering of LiB_xAl_1-_xSi₂O₆ Microwave Dielectric Ceramics with Ultra-low Permittivity

XIONG Siyu¹(), MO Chen¹, ZHU Xiaowei¹, ZHU Guobin¹, CHEN Deqin¹, LIU Laijun¹, SHI Xiaodong², LI Chunchun¹()

1. College of Material Science and Engineering, Guilin University of Technology, Guilin 541004, China
2. College of Physics and Electrical Information Engineering, Guilin University of Technology, Guilin 541004, China

Received:2024-11-27 Revised:2024-12-19 Published:2025-05-20 Online:2025-01-09
Contact: LI Chunchun, associate professor. E-mail: lichunchun2003@126.com
About author:XIONG Siyu (2000-), female, Master candidate. E-mail: xiongsiyu0927@163.com
Supported by:
National Natural Science Foundation of China(62061011)

摘要/Abstract

摘要：

超低介电常数锂基硅酸盐微波介质陶瓷材料作为介质基板在第五代无线通信技术中显示出极大的潜力。然而, 较高的烧结温度带来的残余应力会导致材料的介电损耗增加, 微波介电性能变差。本工作通过在LiAlSi₂O₆陶瓷中引入B³⁺来减少Al³⁺含量, 从而改善LiAlSi₂O₆陶瓷的烧结温度和微波介电性能。采用固相反应法与冷等静压技术相结合的方式制备了LiB_xAl_1-_xSi₂O₆(0≤x≤0.20)微波介质陶瓷, 并研究了B³⁺掺杂对该材料的烧结特性、相结构、微观形貌以及微波介电性能的影响。研究结果表明, 随着掺杂量的增加, 陶瓷的烧结温度由1400 ℃大幅降低至1000 ℃。同时, 相对介电常数(ε_r)从3.95降低至3.69, 品质因数(Q×f)从24300 GHz显著提升至30560 GHz, 谐振频率温度系数(τ_f)从-45.9×10^-6 ℃^-1升高至-20.9×10^-6 ℃^-1。具体而言, ε_r的变化主要受材料本征极化率、晶格振动以及共价键强度的共同影响; Q×f提升则与填充分数(PF)增加和阻尼系数减小密切相关; τ_f增大与氧的键价(V_O)存在较强的关联性。此外, x = 0.20组分展现出最佳的微波介电性能, 具体表现为ε_r = 3.69, Q×f = 30560 GHz, τ_f = -20.9×10^-6 ℃^-1。本研究制备的LiB_xAl_1-_xSi₂O₆为未来高性能微波介质陶瓷材料的开发与应用提供了重要的理论依据和实践指导。

关键词: 超低介电常数, 硅酸铝锂, 微波介电性能

Abstract:

The lithium-based silicate microwave dielectric ceramics with ultra-low permittivity show great potential as substrate materials in the fifth-generation wireless communication technology. However, the residual stress caused by higher sintering temperatures leads to increased dielectric loss, thereby deteriorating the microwave dielectric performance. In this work, B³⁺ was introduced into LiAlSi₂O₆ ceramics to reduce Al³⁺ content, aiming to improve their sintering temperature and microwave dielectric performance. LiB_xAl_1-_xSi₂O₆ (0≤x≤0.20) microwave dielectric ceramics were prepared using a combination of solid-state reaction and cold isostatic pressing techniques. Effects of B³⁺ doping on the sintering characteristics, phase structure, microstructure, and microwave dielectric properties of the materials were characterized. The results show that with a gradual increase in the doping concentration, sintering temperature of the ceramics decreases significantly from 1400 to 1000 ℃. Meanwhile, the relative permittivity (ε_r) decreases from 3.95 to 3.69, the quality factor (Q×f) increases significantly from 24300 to 30560 GHz, and the temperature coefficient of resonant frequency (τ_f) increases from -45.9×10^-6 to -20.9×10^-6 ℃^-1. Specifically, the change in ε_r is mainly influenced by intrinsic polarization, lattice vibrations, and covalent bond strength of the material; the improvement in Q×f is closely related to the increase in packing fraction (PF) and the decrease in damping coefficient; the increase in τ_f is strongly correlated with the bond valence of oxygen (V_O). Furthermore, the composition with x = 0.20 exhibits the best microwave dielectric performance with ε_r = 3.69, Q×f = 30560 GHz, and τ_f = -20.9×10^-6 ℃^-1. Findings of this study on LiB_xAl_1-_xSi₂O₆ provide important theoretical guidance and practical insights for development and application of high-performance microwave dielectric ceramics in the future.

Key words: ultra-low permittivity, lithium aluminum silicate, microwave dielectric property

中图分类号:

TQ174

熊思宇, 莫尘, 朱肖伟, 朱国斌, 陈德钦, 刘来君, 施晓东, 李纯纯. 超低介电常数LiB_xAl_1-_xSi₂O₆微波介质陶瓷的低温烧结[J]. 无机材料学报, 2025, 40(5): 536-544.

XIONG Siyu, MO Chen, ZHU Xiaowei, ZHU Guobin, CHEN Deqin, LIU Laijun, SHI Xiaodong, LI Chunchun. Low-temperature Sintering of LiB_xAl_1-_xSi₂O₆ Microwave Dielectric Ceramics with Ultra-low Permittivity[J]. Journal of Inorganic Materials, 2025, 40(5): 536-544.

图/表 10

图1 LiAlSi2O6的晶体结构

Fig. 1 Crystal structure of LiAlSi2O6

图2 LiBxAl1-xSi2O6陶瓷的XRD图谱

Fig. 2 XRD patterns of LiBxAl1-xSi2O6 ceramics (a) At the optimum sintering temperature; (b-d) Rietveld refinement fitting patterns at (b) x = 0, (c) x = 0.12, and (d) x = 0.20

表1 LiBxAl1-xSi2O6陶瓷的Rietveld结构精修参数

Table 1 Rietveld refined structural parameters of LiBxAl1-xSi2O6 ceramics

x	Lattice parameter				$R p$ /%	$R wp$ /%	χ²
x	a/nm	b/nm	c/nm	V/nm³	$R p$ /%	$R wp$ /%	χ²
0	0.75380(5)	0.75380(5)	0.91556(4)	0.52024(4)	7.69	10.8	1.84
0.05	0.75346(3)	0.75346(3)	0.91533(1)	0.51963(9)	7.32	10.1	1.83
0.08	0.75320(5)	0.75320(5)	0.91494(0)	0.51906(2)	7.24	10.2	1.89
0.12	0.75286(8)	0.75286(8)	0.91434(9)	0.51826(2)	7.24	10.2	1.87
0.16	0.75246(2)	0.75246(2)	0.91332(8)	0.51712(5)	7.29	10.1	1.86
0.20	0.75206(4)	0.75206(4)	0.91257(9)	0.51615(5)	7.22	9.98	1.87

表1 LiBxAl1-xSi2O6陶瓷的Rietveld结构精修参数

Table 1 Rietveld refined structural parameters of LiBxAl1-xSi2O6 ceramics

x	Lattice parameter				$R p$ /%	$R wp$ /%	χ²
x	a/nm	b/nm	c/nm	V/nm³	$R p$ /%	$R wp$ /%	χ²
0	0.75380(5)	0.75380(5)	0.91556(4)	0.52024(4)	7.69	10.8	1.84
0.05	0.75346(3)	0.75346(3)	0.91533(1)	0.51963(9)	7.32	10.1	1.83
0.08	0.75320(5)	0.75320(5)	0.91494(0)	0.51906(2)	7.24	10.2	1.89
0.12	0.75286(8)	0.75286(8)	0.91434(9)	0.51826(2)	7.24	10.2	1.87
0.16	0.75246(2)	0.75246(2)	0.91332(8)	0.51712(5)	7.29	10.1	1.86
0.20	0.75206(4)	0.75206(4)	0.91257(9)	0.51615(5)	7.22	9.98	1.87

图3 LiBxAl1-xSi2O6陶瓷的密度与烧结温度的关系

Fig. 3 Relationship between bulk density and sintering temperature of LiBxAl1-xSi2O6 ceramics (a) LiAlSi2O6 ceramic; (b) LiBxAl1-xSi2O6 ceramic; (c) Bulk density and sintering temperature varied with x

图4 LiBxAl1-xSi2O6陶瓷的SEM照片和晶粒尺寸分布

Fig. 4 SEM images and grain size distributions of LiBxAl1-xSi2O6 ceramics (a) x = 0; (b) x = 0.05; (c) x = 0.08; (d) x = 0.12; (e) x = 0.16; (f) x = 0.20

图5 LiBxAl1-xSi2O6陶瓷的拉曼光谱图及性能参数

Fig. 5 Raman spectra and corresponding parameters of LiBxAl1-xSi2O6 ceramics (a) Raman spectra at different compositions; (b) Raman shift and FWHM at 493 cm-1 changed with composition

图6 LiBxAl1-xSi2O6陶瓷的微波介电性能

Fig. 6 Microwave dielectric properties of LiBxAl1-xSi2O6 ceramics (a) εr and εcorr; (b) Q×f and PF; (c) τf and VO

表2 LiBxAl1-xSi2O6陶瓷样品的Vm、α、εtheo、εr和α/Vm

Table 2 Vm, α, εtheo, εr, and α/Vm of LiBxAl1-xSi2O6 ceramics

x	V_m / nm³	α / nm³	ε_theo	ε_r	α·V_m^-1
0	0.1300610	0.0157900	4.1042	3.95	0.121405
0.05	0.1299098	0.0157530	4.0968	3.90	0.121261
0.08	0.1297655	0.0157308	4.0949	3.85	0.121225
0.12	0.1295655	0.0157012	4.0928	3.81	0.121184
0.16	0.1292813	0.0156716	4.0947	3.76	0.121221
0.20	0.1290388	0.0156420	4.0946	3.69	0.121219

表3 LiBxAl1-xSi2O6陶瓷的键价、共价键强度和平均共价键强度

Table 3 Bond valence, covalence and average covalence of LiBxAl1-xSi2O6 ceramics

x	V_Li	V_Si/Al	V_O	C_Li-O/%	C_Si/Al-O/%	Average/%
0	0.820	3.906	1.912	18.87	53.18	36.03
0.05	0.821	3.935	1.924	18.89	53.44	36.16
0.08	0.823	3.947	1.930	18.92	53.54	36.23
0.12	0.824	3.978	1.943	18.94	53.81	36.37
0.16	0.825	4.036	1.968	18.95	54.31	36.63
0.20	0.829	4.075	1.986	19.02	54.65	36.83

表4

Table 4 Sintering temperatures (ST) and microwave dielectric properties of several silicates compared with LiBxAl1-xSi2O6[17,19,26,28,38,41 -45]

Component	ST/℃	ε_r	Q×f/GHz	τ_f/(×10^-6, ℃^-1)	Ref.
LiAlSiO₄	1350	4.9	36000	-57.3	[17]
Li(Al_0.99Li_0.01)SiO_3.99	1250	3.49	51358	-51.48	[17]
Ca₂SiO₄	1450	8.6	26100	-89	[19]
Sr₂SiO₄	1575	9.5	19100	-205	[19]
Ba₂SiO₄	1525	13.1	17900	-17	[19]
Zn₂SiO₄	1340	5.7	53000	-16	[41]
Ba₂ZnSi₂O₇	1200	8.09	26600	-51.4	[42]
Sr₂MgSi₂O₇	1280	6.85	22530	-32	[43]
Sr₃MgSi₂O₈	1450	11.6	25375	-57.41	[44]
Li₂SiO₃	1025	6.19	30550	-40.95	[38]
Li₂ZnSiO₄	1250	5.8	14700	-96.6	[45]
Li₂MgSiO₄	1100	5.73	13570	-16.7	[26]
LiB_xAl_1-_xSiO₄(0.02≤x≤0.1)	875-1100	3.34-3.73	25770-27540	-22.85--16.5	[28]
LiB_xAl_1-_xSi₂O₆(0≤x≤0.20)	1000-1400	3.69-3.95	24300-30500	-45.9--20.9	This work

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超低介电常数LiB_xAl_1-_xSi₂O₆微波介质陶瓷的低温烧结

Low-temperature Sintering of LiB_xAl_1-_xSi₂O₆ Microwave Dielectric Ceramics with Ultra-low Permittivity

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[4]	张瑶, 丁士华, 刘杨琼, 段绍英, 肖鹏, 韩林材. Ba_1-_xMg_xAl₂Si₂O₈晶体结构与微波介电性能的研究[J]. 无机材料学报, 2017, 32(1): 91-95.
[5]	张康, 李蔚, 林慧兴. MgO/Eu₂O₃共掺杂对Al₂O₃陶瓷微波介电性能的影响[J]. 无机材料学报, 2015, 30(9): 984-988.
[6]	苏静杰, 杨梓, 李义锋, 唐伟忠, 安晓明, 郭辉. 分体圆柱谐振腔法用于金刚石膜微波介电性能测试的研究[J]. 无机材料学报, 2015, 30(7): 751-756.
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[9]	雷文,吕文中,王晓川,梁军,江建军. CaTiO₃对(1-x)ZnAl₂O₄-xMg₂TiO₄(x=0.21)微波介质陶瓷结构和性能的影响[J]. 无机材料学报, 2009, 24(5): 957-961.
[10]	刘忠池,周东祥,龚树萍,胡云香. 铜钼复合添加ZnO-TiO₂微波介质陶瓷的低温烧结及相转变[J]. 无机材料学报, 2009, 24(4): 712-716.
[11]	李月明,宋婷婷,胡元云,彭浩,刘维良. (1-x)CaTiO_3-xLi_1/2Sm_1/2TiO₃陶瓷的微波介电性能研究[J]. 无机材料学报, 2008, 23(4): 695-699.
[12]	王焕平,徐时清,张启龙,杨辉. 溶胶-凝胶制备(Ca_0.7Mg_0.3)SiO₃陶瓷及其微波介电性能[J]. 无机材料学报, 2008, 23(4): 691-694.
[13]	吕文中,朱建华,Eric Rop Kipkoech. NdAlO₃掺杂对Ba_4.2Nd_9.2Ti₁₈O₅₄陶瓷微波介电性能的影响[J]. 无机材料学报, 2006, 21(1): 139-144.
[14]	胡明哲,周东祥,姜胜林,蔡雪卿,黄静. Nd³⁺取代对(PbCa)(FeNb)O₃介质陶瓷微波特性及晶体结构的影响研究[J]. 无机材料学报, 2005, 20(1): 126-132.
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