熊洁羽等：K2SO4辅助混合模板剂制备大孔–中孔SiO2微球· 2331 ·第38卷第12期氟氧微晶玻璃/二氧化硅系低温共烧陶瓷材料的煅烧行为王阳培华1,2，齐西伟2，李勃1,4，戴春雷3，郭海3，周济4(1. 清华大学深圳研究生院，广东深圳 518055；2. 东北大学秦皇岛分校，河北秦皇岛 066004；3. 深圳顺络电子股份有限公司，广东深圳 518110；4. 清华大学材料科学与工程系，新型陶瓷与精细工艺国家重点实验室，北京 100084)摘要：制备SiO2–B2O3–Al2O3–AlF3–Li2O–Na2O–K2O–CaO系氟氧低温微晶玻璃/二氧化硅共烧陶瓷材料，用X射线衍射、扫描电子显微镜和阻抗分析仪分析讨论氟氧微晶玻璃/氧化硅主晶相的形成、致密性及介电性能。结果表明：氟氧玻璃/氧化硅陶瓷材料体系样品的最佳煅烧温度范围为750～780℃，煅烧时部分玻璃相转变成方石英，有助于进一步降低相对介电常数(εr)和介电损耗(tanδ)，在780℃煅烧时，样品的体积密度达到最大值(2.31g/cm–3)，此时在1GHz频率测试，εr=4.42，tanδ=3×10–3，所制备的材料是一种在基板、无源集成和电子封装等方向都具有较大应用前景的低温共烧陶瓷材料。关键词：氟氧微晶玻璃；低温共烧陶瓷；玻璃陶瓷；介电性能中图分类号：O482.3 文献标志码：A 文章编号：0454–5648(2010)12–2331–04CALCINING BEHA VIOR OF OXYFLUORIDE GLASS-CERAMICS/SILICON DIOXIDESYSTEM FOR LTCCWANGYANG Peihua1,2，QI Xiwei2，LI Bo1,4，DAI Chunlei3，GUO Hai3，ZHOU Ji4(1. Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055, Guangdong; 2. Northeastern University at QinhuangdaoBranch, Qinhuangdao 066004, Hebei; 3. Shenzhen Sunlord Electronics Cooperation Limited, Shenzhen 518110, Guangdong;4. State Key Laboratory of New Ceramics and Fine Processing, Department of Materials Science and Engineering,Tsinghua University, Beijing 100084, China)Abstract: A SiO2–B2O3–Al2O3–AlF3–Li2O–Na2O–K2O–CaO low temperature co-fired oxyfluoride glass-ceramics/silicon dioxide system was prepared. The phase transition behavior, density and dielectric properties were studied by the X-ray diffraction, scanning electron microscopy and impedance analysis. The results show that the best calcining temperature range for this system is 750–780℃.The relative dielectric constant (εr) and dielectric loss(tanδ) of the oxyfluoride glass-ceramics/silicon dioxide system decrease with the increasing of sintering temperature because part of the amorphous glass phase is transformed into cristobalite phase. The sample reaches the maximum bulk density (2.31g/cm3), and the εr decreases to 4.42. The tanδalso falls to approximately 3×10–3 at 1GHz when the samples are calcined at 780℃. The system is promising as a candidate for a new dielectric material for low temperature co-fired ceramic substrate, passive integration and packaging technology.Key words: oxyfluoride glass-ceramics; low temperature co-fired ceramic; glass-ceramic; dielectric properties近年来，随着电子信息技术的飞速发展，对电子元器件微型化、集成化和高频化的要求不断提高。在制作多层元件或把无源器件埋入多层电路基板中的过程中，选择适当的能与银等导电材料在低温(低于900℃)实现共烧[1–2],[3]21–23的电子封装材料，成为上述研究的关键。目前在众多的封装技术中，利用低温共烧陶瓷(low temperature co-fired ceramic，LTCC)技术制备的片式无源集成器件不仅具备高频高品质特性，而且还具备高可靠性、优良的电性能和密封性能。[1,4–6]目前，高频低介电常数电子封装陶瓷由于有利于提高信号的传输速率、降低信号的延迟时间而成收稿日期：2010–04–05。修改稿收到日期：2010–07–28。基金项目：国家自然科学基金(50902081)，国家“973”计划(2009CB62- 3304)，国家“863”计划(2007AA03Z449)和广东省省部产学研(2009A090100021)资助项目。第一作者：王阳培华(1983—)，男，硕士研究生。通信作者：李勃(1976—)，男，博士，副教授。Received date:2010–04–05. Approved date: 2010–07–28.First author: WANGYANG Peihua (1983–), male, graduate student for master degree.E-mail: wangyangpeihua@hotmail.comCorrespondent author: LI Bo (1976–), male, Doctor, associate professor.E-mail: boli@mail.tsinghua.edu.cn第38卷第12期2010年12月硅酸盐学报JOURNAL OF THE CHINESE CERAMIC SOCIETYVol. 38，No. 12December，2010
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