Article(id=1321944758738596723, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1321944712408314326, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250457, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1749484800000, receivedDateStr=2025-06-10, revisedDate=1751558400000, revisedDateStr=2025-07-04, acceptedDate=null, acceptedDateStr=null, onlineDate=1793105791028, onlineDateStr=2026-10-27, pubDate=1773936000000, pubDateStr=2026-03-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793105791028, onlineIssueDateStr=2026-10-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793105791028, creator=13701087609, updateTime=1793105791028, updator=13701087609, issue=Issue{id=1321944712408314326, tenantId=1146029695717560320, journalId=1263187385517883426, year='2026', volume='54', issue='3', pageStart='821', pageEnd='1176', issueExtLink='null', onlineDate='null', pubDate='1770652800000', pubDateStr='2026-02-10', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793105779983, creator='13701087609', updateTime=1793105779983, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=1042, endPage=1051, ext={EN=ArticleExt(id=1321944759250301812, articleId=1321944758738596723, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Effects of Cu
2+ Substitution and LiF Additive on Low-Temperature Sintering and Microwave Performance of CoTi
0.2Zr
0.8Nb
2O
8 Ceramics, columnId=1263922769897599102, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Articles, runingTitle=null, highlight=null, articleAbstract=
Introduction A2+B4+Nb2O8-type ceramics (where A = Co, Ni, Zn and B = Ti, Zr) are critical materials for satellite communication and mobile base station applications due to their moderate relative permittivity (εr) and high-quality factor (Q × f). Among these, CoTi0.2Zr0.8Nb2O8 ceramic demonstrates superior microwave dielectric properties (i.e., εr of 26.5, Q × f value of 76921 GHz, and τf of-15×10-6/℃). However, its high sintering temperature (1350 ℃) has a major challenge for practical implementation in low-temperature co-fired ceramic (LTCC) systems, where lower processing temperatures are essential for compatibility with silver electrodes and multilayer integration. This study was to prepare CuxCo1-xTi0.2Zr0.8Nb2O8 (0.0≤x≤0.3) ceramic system via the partial substitution of Co2+ ions with Cu2+ ions and LiF flux doping. The optimal Cu2+ substitution level was determined via the systematic analysis of the quality factor (Q × f) of ceramics with varying compositions. LiF was introduced as a sintering aid, effectively reducing the sintering temperature of Cu0.2Co0.8Ti0.2Zr0.8Nb2O8 ceramic. The results demonstrated that Cu0.2Co0.8Ti0.2Zr0.8Nb2O8 ceramic with 30% LiF additive, sintered at 950 ℃ exhibited a superior compatibility with silver electrodes and achieved optimal microwave dielectric properties (i.e., a relative permittivity (εr) of 30, a high Q × f value of 44,571 GHz, and a temperature coefficient of resonant frequency (τf) of -42.0×10-6/℃).
Methods The raw materials were precisely weighed according to stoichiometric ratios and subjected to ball milling in a horizontal ball mill with zirconia balls with ethanol as a dispersant for 24 h. The resulting slurry was dried at 85 ℃ for 4 h and calcined at 900 ℃ for 3 h. Afterwards, the powders were further ground in the mill under identical conditions for 24 h to ensure the material homogeneity. After subsequent drying at 85 ℃ for 4 h and sieving through a 40-mesh screen, the finer powders were mixed with 5%PVA as a binder in an agate mortar, passed through a 200-mesh sieve, and uniaxially pressed into green pellets with 10 mm diameter× 5 mm height. These pellets were first debindered at 600 ℃ for 2 h before being sintered between 1200-1300 ℃ for 4 h. For low-temperature sintering optimization, LiF at different concentrations (i.e., 0-40.0%, 99.9% purity, Macklin Biochemical Co.) was introduced during secondary milling, and the modified samples were prepared under the same processing condictions but sintered at a reduced temperature of 950 ℃ for 4 h.
Results and discussion This study obtains a low-temperature sintering and performance optimization of CuxCo1-xTi0.2Zr0.8Nb2O8 (0.0≤x≤0.3) ceramics via a strategy of partial Cu2+ substitution for Co2+ and LiF flux doping. The XRD patterns confirm the effective solid solution of Cu2+ without secondary phase formation, though the lattice contraction appears due to the smaller ionic radius of Cu2+ (i.e., 0.73 Å), compared to Co2+ (i.e., 0.74 Å). The sample with x of 0.2 demonstrates an optimal comprehensive performance.
For the introduction of LiF as a flux agent, the sintering temperature of Cu0.2Co0.8Ti0.2Zr0.8Nb2O8 can be reduced from 1200 ℃ to 950 ℃. The Rietveld refinement indicates the formation of a (Li, Cu)NbO3 secondary phase, and the content increases at a higher LiF doping concentration (i.e., 10%-40%). The SEM images show that the 30% LiF-doped sample has the most homogeneous microstructure (grain size: 0.52 ± 0.12 μm) and a high relative density, leading to an optimal microwave property (i.e., εr = 30, Q × f=44,571 GHz, and τf = -42.0×10-6/℃). The results of Co-firing experiments confirm an excellent chemical compatibility between the 30% LiF-doped ceramic and silver electrodes at 950 ℃ without any interfacial reactions.
Conclusions This study prepared CuxCo1-xTi0.2Zr0.8Nb2O8 (0.0≤x≤0.3) ceramic system via the partial substitution of Co2+ ions with Cu2+ ions and LiF flux doping, enabling dense sintering at 950 ℃. The optimal 30% LiF-doped Cu0.2Co0.8Ti0.2Zr0.8Nb2O8 ceramic sintered at 950 ℃ for 4 h achieved an exceptional performance (i.e., εr = 30, Q × f = 44,571 GHz, and τf = -42.0×10-6/℃) with an excellent Ag electrode compatibility, demonstrating a promising potential for microwave dielectric applications.
, authors=Qi QU
1, Xinghua MA
1, Zhenlu ZHANG
2, authorsList=Qi QU, Xinghua MA, Zhenlu ZHANG, authorCompany=null, correspAuthors=Xinghua MA, authorNote=
, correspAuthorsNote=
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0.2Zr
0.8Nb
2O
8陶瓷低温烧结及微波性能的影响, columnId=1263922770220560512, journalTitle=硅酸盐学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
A2+B4+Nb2O8体系（A = Co、Ni、Zn等；B = Ti、Zr等）因优异的微波介电性能备受关注，但烧结温度过高，严重阻碍其在LTCC领域的应用。本工作采用Cu2+部分置换Co2+的策略，成功制备了CuxCo1-xTi0.2Zr0.8Nb2O8（0.0≤x≤0.3）陶瓷体系。通过系统分析不同组分陶瓷的品质因数（Q × f），确定Cu2+最优置换量（x = 0.2）。在此基础上，进一步引入LiF作为烧结助剂，成功将Cu0.2Co0.8Ti0.2Zr0.8Nb2O8陶瓷的烧结温度降低至950 ℃。结果表明，添加30%（摩尔分数）LiF的Cu0.2Co0.8Ti0.2Zr0.8Nb2O8陶瓷在950 ℃烧结温度下不仅表现出优异的银电极兼容性，同时展现出最优的微波介电性能：εr = 30，Q × f = 44, 571 GHz，τf = -42.0×10-6/℃。
, authors=曲奇
1, 马兴华
1, 张振路
2, authorsList=曲奇, 马兴华, 张振路, authorCompany=null, correspAuthors=马兴华, authorNote=
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马兴华（1985—），男，博士，副教授。
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