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1、合肥工业大学 硕士学位论文 用于LTCC的微晶玻璃的制备及其性能研究 姓名：王敏 申请学位级别：硕士 专业：材料物理与化学 指导教师：左如忠 2010-09 用于用于 LTCC 的微晶玻璃的制备及性能研究的微晶玻璃的制备及性能研究 摘摘 要要 在混合集成电路技术基础上发展起来的多芯片互联技术对材料提出了更高 的要求，低温共烧陶瓷（LTCC）因其集成密度高、高频特性好等独特的优势成 为近年来微电子封装界备受瞩目的组件整合技术。CaO- B2O3- SiO2系微晶玻璃 是硅灰石型微晶玻璃体系的一种，硅灰石本身的介电常数与介电损耗均较低， 因而是用于 LTCC 最有前途的组成体系之一， 在封装材料中
2、有很好的应用前景。 本文采用溶胶凝胶法制备了钙硼硅粉体，这种工艺避免了在熔融法和固相 法中由于高温熔融时低熔点组元 B 在高温下挥发而引起的组分偏移；而且溶胶 凝胶工艺制备的粉体纯度高、组分均匀。研究了合成过程中溶胶凝胶的水解、 聚合机理，以及凝胶在热处理过程中的结构演变。结果表明，在酸性条件下， 溶胶至凝胶的反应过程通过亲电取代得以进行，形成了以SiO4、BO3为基本 单位的三维网络结构，Ca2+则均匀的填充在空隙之中。凝胶通过热处理形成了 稳定的 Si- O- B 键，且此时内部结构更加有序，从而使析晶时分子之间调整的间 距减小。最佳核化和晶化制度由一系列实验确定，本文确定晶化制度为 80
3、0900oC2h，核化制度为 680oC3h。 根据 CaO- B2O3- SiO2三元相图设计了六个组成，采用预先确定的最佳烧结 温度对玻璃粉体经过核化和晶化使之成为微晶玻璃，其主晶相为 CaSiO3、 CaB2O4，介电常数 r=3.55.5，介电损耗 tan=0.00090.004，且微晶玻璃的烧 结致密化及介电性能与各个组分的含量具有很强的依赖性。Ca 是网络外体，适 量的 Ca 是晶相的主要成分，过多的 Ca 会导致介电损耗的增大；Si 和 B 是网络 形成体，过多 Si 的存在会使烧结温度偏高，而 B 的存在则会使体系液相增多， 促进烧结。因而 800900oC 之间烧结后组分为
4、40CaO- 20B2O3- 40SiO2的微晶玻 璃具有最优的性能，介电常数 r=4.83，介电损耗 tan=0.00089。 由于微晶玻璃易受到热处理制度的影响，在 CaO- B2O3- SiO2体系中添加不 同量先行合成的 CaSiO3陶瓷相， 研究它对 CaO- B2O3- SiO2微晶玻璃体系的析晶 行为、烧结致密化、微观结构、介电性能等的影响规律。研究表明，CaSiO3在 烧结初期中起到诱导、促进析晶的作用，并与 CaO- B2O3- SiO2体系中生成的 CaSiO3实现了很好的互溶，从而使体系的结构更为紧凑，致密化程度增加。 CaSiO3的添加量有个最佳值，当 CaSiO3含量
5、为 10%时，1MHz 下于室温测得的 介电常数 r=5.06，介电损耗 tan=0.00064。 关键词：关键词：LTCC；微晶玻璃；CaO- B2O3- SiO2；溶胶凝胶法；介电性能 Research on Preparation and Properties of Glass-Ceramic for LTCC ABSTRACT With the development of hybrid IC technique, further requests for materials have been put forward. Recently, low temperature co- fi
6、red ceramics (LTCC) technology is the most attractive multi- chip integrated method which has such advantages as low cost, space- saving and high density. CaO- B2O3- SiO2 (CBS) system belongs to one wollastonite- type glass- ceramic and has achieved industrial application in electronic package field
7、s because it has excellent electrical properties and low- temperature co- firable characteristics. A sol- gel soft chemical route was used to prepare CaO- B2O3- SiO2 glass powder, not only avoid the B volatilizing under high melting temperature in conventional way to prepare CBS glass powder, but al
8、so obtain more pure and uniformity powders. This paper is focused on the mechanism of hydrolyze and polymerization and the structural evolution in xerogel at various heat- treat temperatures. The xerogel exhibits SiO4 or BO3 based three- dimensional network structure whose interstices Ca ions fill i
9、n, which becomes more orderly and stable after heat treatments, for the formation of Si- O- B bond made the adjustment between molecules smaller in devitrification. Six compositions of CaO- B2O3- SiO2 system were designed in this research based on the phase diagram. The glass- ceramics are obtained
10、with CaSiO3 and CaB2O4 phases through the nucleation and crystallization processes which are predefined by experiments. After sintered at 800- 900oC, their dielectric properties at 1MHz of as- sintered glass- ceramics are r=5.15 and tan=0.00095, respectively. Ca is the bases of main phase, excess wi
11、ll lead to the increase of dielectric loss. Si and B is the network former, too much Si in existence will result in a higher sintering temperature and suitable B will promote sinter for forming more liquid phase. The results indicate that the densification and dielectric property are strongly depend
12、ent on the content of each component. So the most excellent dielectric constant of the six is 4.83, corresponding the dielectric loss is 0.00089. In order to relieve the influence of sintering on glass- ceramic, investigation on the densification properties, structure and dielectric properties of th
13、e CaO- B2O3- SiO2 glasses + CaSiO3 crystalline ceramic were performed in this study. The result shows that CaSiO3 plays a role on inductive and improve crystallization when the content of CS is small, which promotes the densification of glass+ceramic. The glass phase and ceramic phase are homogeneou
14、s mixed to a certain extent for the samples structure is more compact consequently. When a sintering temperature is 850 oC with the CBS:CS=1:9, the optimum dielectric properties are obtained with the dielectric constant r is 5.06 and the dielectric loss tan is 0.00064 at 1MHz. Keywords: LTCC; Glass Ceramic; CaO- B2O3- SiO2; Sol- Gel; Dielectric properities 插图清单插图清单 图 1- 1 典型的 LTCC 基板 .1 图 1- 2 LTCC 技术与厚膜工艺及 HTCC 技术的比较.2 图 1- 3 LTCC 器件应用领域所占比例 .3 图 1- 4 全球 LTCC 厂商市场占有情况图.3 图 1- 5 全球 RF 元件/模组市场规模预测 .3 图 2- 1 溶胶- 凝胶法制备 CaO- B2O3- SiO2玻璃粉体工艺流程图 .15 图 2- 2 溶胶凝胶反应过程微观示意图 .16 图 2- 3 溶胶和凝胶的红外光谱图.
