复合双性LTCC材料基础研究
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摘要
随着电子技术在自动化、工业控制、医学、航天航空和日常生活等领域的广泛应用，高密度、宽温域、小尺寸、多功能、高品质等特性日益成为其发展的必然趋势，同时这些特性给传统封装技术及工艺带来了巨大的挑战。在众多的封装技术中，低温共烧陶瓷LTCC(Low Temperature Co-fired Ceramic)技术成为了国际研究的焦点，因为利用LTCC技术制备的产品不仅能具备高电流密度、小体积，而且还具备高可靠性和优良的电性能、传输特性及密封性。
LTCC技术是一种先进的混合电路封装技术。它将四大无源器件，即变压器(T)、电容器(C)、电感器(L)、电阻器(R)集成，配置于多层布线基板中，与有源器件(如：功率MOS、晶体管、IC电路模块等)共同集成为一完整的电路系统。因此LTCC技术又称为混合集成技术，它能有效地提高电路的封装密度及系统的可靠性。
本文围绕LTCC技术中的低温共烧铁氧体LTCF(Low Temperature Co-fired Ferrite)材料采用理论、实验及应用三位一体的研究模式，开发了一种新型LTCC复合介质材料，不但对该材料的复合机理进行了理论模拟而且对其在LTCC滤波器中的应用展开了研究。本论文在理论模型、材料制备和器件设计上做了一些探索性和创新性的工作，具体内容如下：
一、探索性地建立了针对LTCC陶瓷的低温烧结模型：模型基于液相烧结理论，以液相在晶粒边界引起的毛细管压力及溶解-淀析过程中化学势能的变化为烧结驱动力，将烧结温度、时间与烧结后的最终晶粒大小、相对密度联系起来，模拟出低温烧结动态过程中相对密度的变化趋势。
二、首次提出铁电—铁磁复合材料的复合理论并给予了系统的分析：讨论了复合材料中两相成分的化学结构及电磁性能在理论上对复合可能性的影响，根据材料的微观结构建立了复合模型，模型中假设铁电相均匀分布于铁磁相晶粒表面，并和气孔一起形成非磁性薄层将铁磁晶粒之间隔断，使铁磁颗粒孤立。通过对复合结构中铁磁晶粒内场变化的分析，推导出复合材料铁电／铁磁成分比与复合磁导率的关系方程；另外，利用微观结构中电流流通的等效电路，推导得到不同铁电／铁磁成分比时复合材料复数介电常数与频率的关系表达式。
三、研究了工艺条件对材料电磁性能的影响：按照工艺流程改变工艺参数预烧温度、二次球磨时间、烧结曲线中升温降温速度、烧结温度和保温时间，通过电镜扫描SEM、X射线衍射等分析手段了解改变工艺参数对铁氧体材料微观结构的影响规律，通过对材料介电常数频谱、磁导率频谱及品质因数的测量得知工艺参数对材料电磁性能的影响规律，根据实验数据结果得到最佳铁氧体烧结工艺参数。
四、研究了不同掺杂离子及助熔剂的加入对低温烧结铁氧体LTCF材料的微观结构及电磁性能影响：首先研究了不同MnCO_3和CuO含量对NiZn铁氧体烧结特性、微观结构及电磁性能的影响，首次发现了掺杂Mn离子的NiZn铁氧体其电磁性能对烧结温度具有敏感性。其次研究了不同助熔剂Bi_2O_3、WO_3和Nb_2O_5对NiCuZn铁氧体烧结特性、微观结构及电磁性能的影响，实验揭示W~(6+)离子对材料微观结构的改善；最后对低温NiCuZn铁氧体进行改性掺杂，研究稀土氧化物CeO_2对其微观结构及电磁性能的影响，并给出NiCuZn铁氧体掺杂稀土元素时的磁频谱及介频谱。
五、开发了一新型的基于不同低温烧结NiCuZn铁氧体与高介电常数(BaTiO_k+X)钙钛矿的具有电感、电容双性的铁电—铁磁复合材料，研究了不同铁电—铁磁含量对各组复合材料微观结构及电容电感双性的影响。并研究了不同助熔剂Bi_2O_3、WO_3和Nb_2O_5对其烧结特性、微观结构及电容电感双性的影响。最后对复合材料进行稀土掺杂改性，研究稀土氧化物CeO_2对其微观结构及电容电感双性的影响。
六、设计并制作出两种使用第六章LTCC复合双性材料的3G通讯设备用带通滤波器，采用Ansoft HFSS电磁仿真软件对所建立的滤波器模型进行模拟仿真，通过调节滤波器结构参数使滤波器各性能指标达到目标要求，并实现生产制备。制得带通中心频率3.5GHz，插损＜2.8dB，带宽＞400MHz，阻带衰减大于35dB的微带式带通滤波器和带通中心频率1.4GHz，插损＜3dB，带宽＞160MHz，阻带衰减大于30dB的LC式带通滤波器。
New electronic systems fo automotive/industrial/medical/aerospace will continue to challenge both packaging engineers and technology due to the increased performance requirements, higher densities, higher temperatives and limited space available. This challenge mandates the use of unique packaging techniques such as Low Temperature Co-fired Ceramic (LTCC) technology that must not only provide the increase circuit density but also the reliability, electrical and medical performance, thermal management, and hermeticity.
Low Temperature Co-fired Ceramic (LTCC) technology is a new packaging technology for integrate circuit, which consists of buried passive devices such as transformer, conductors, resistors, and capacitors in the multilayer of module and can easily integrate with active devices such as power MOS, transistors, and IC module. Recently, this technology was widely focused and researched for its wonderful properties.
Focused on the LTCC materials, we carried through some researches as follows:
1. A low temperature sintering model was established based on the liquid sintering theories. The sintering temperature and sintering time dependence of relative density for the sintered ceramics were simulated.
2. With the systemically analyses of the synthesis of ferroelectric-ferromagnetic composite materials, the low temperature sintered NiCuZn ferrites and perovskite BaTiO_k+X was chosen as the main components. A model was given by assuming the isolation of magnetic grains by surrounding non-magnetic layer to evaluate the internal field and the complex permeability of whole material as a function of the ratio of perovskite content to ferrite content.
3. We researched the effects of preparation process on the microstructure and electromagnetic properties of ceramics. The pre-sintering temperature, milling time, firing rate, sintering temperature, and holding time are changed regularly to investigate the variation of the phase formation by X-ray diffraction studies, the micrographs of the sintered ceramics by SEM, and the bulk density by Archimedes method. The frequency dependence of complex permeability, quality factor, and dielectric constant are studied.
4. The effects of sintering temperature and Mn ions contents on the microstructure and electromagnetic properties of NiZn ferrites are studied. To decreased the sintering temperature, CuO was introduced in NiZn ferrites first, and then the flux oxides such as Bi_2O_3, WO_3, and Nb_2O_5 are introduced in NiCuZn ferrites.
The variation of microstructure and electromagnetic properties with these reducing-sintering-temperature oxides' content are investigated. Finally, we researched the influence of rare earth ions Ce~(4+) on low temperature sintered NiCuZn ferrites.
5. A new ferroelectric-ferromagnetic composite material is synthesized by usual ceramic technology with NiCuZn ferrites and perovskite BaTiO_k+X as the main components. The microstructure and electromagnetic properties of the composite with different composition of NiCuZn ferrites and different perovskite contents are investigated. After that, the influences of flux oxide Bi_2O_3, WO_3, and Nb_2O_5 and the Ca~(2+), Ce~(4+) ions on this composite material are also studied.
6. A LTCC band pass filter is designed with this composite material using the Ansoft HFSS software. This filter has insertion loss in the pass band < -2.8dB, the attenuation losses in the stopband were more than 40 dB, the centre frequency of the pass band is 1.9GHz and the 3 dB band width is more than 200MHz.
LTCC技术是一种先进的混合电路封装技术。它将四大无源器件，即变压器(T)、电容器(C)、电感器(L)、电阻器(R)集成，配置于多层布线基板中，与有源器件(如：功率MOS、晶体管、IC电路模块等)共同集成为一完整的电路系统。因此LTCC技术又称为混合集成技术，它能有效地提高电路的封装密度及系统的可靠性。
本文围绕LTCC技术中的低温共烧铁氧体LTCF(Low Temperature Co-fired Ferrite)材料采用理论、实验及应用三位一体的研究模式，开发了一种新型LTCC复合介质材料，不但对该材料的复合机理进行了理论模拟而且对其在LTCC滤波器中的应用展开了研究。本论文在理论模型、材料制备和器件设计上做了一些探索性和创新性的工作，具体内容如下：
一、探索性地建立了针对LTCC陶瓷的低温烧结模型：模型基于液相烧结理论，以液相在晶粒边界引起的毛细管压力及溶解-淀析过程中化学势能的变化为烧结驱动力，将烧结温度、时间与烧结后的最终晶粒大小、相对密度联系起来，模拟出低温烧结动态过程中相对密度的变化趋势。
二、首次提出铁电—铁磁复合材料的复合理论并给予了系统的分析：讨论了复合材料中两相成分的化学结构及电磁性能在理论上对复合可能性的影响，根据材料的微观结构建立了复合模型，模型中假设铁电相均匀分布于铁磁相晶粒表面，并和气孔一起形成非磁性薄层将铁磁晶粒之间隔断，使铁磁颗粒孤立。通过对复合结构中铁磁晶粒内场变化的分析，推导出复合材料铁电／铁磁成分比与复合磁导率的关系方程；另外，利用微观结构中电流流通的等效电路，推导得到不同铁电／铁磁成分比时复合材料复数介电常数与频率的关系表达式。
三、研究了工艺条件对材料电磁性能的影响：按照工艺流程改变工艺参数预烧温度、二次球磨时间、烧结曲线中升温降温速度、烧结温度和保温时间，通过电镜扫描SEM、X射线衍射等分析手段了解改变工艺参数对铁氧体材料微观结构的影响规律，通过对材料介电常数频谱、磁导率频谱及品质因数的测量得知工艺参数对材料电磁性能的影响规律，根据实验数据结果得到最佳铁氧体烧结工艺参数。
四、研究了不同掺杂离子及助熔剂的加入对低温烧结铁氧体LTCF材料的微观结构及电磁性能影响：首先研究了不同MnCO_3和CuO含量对NiZn铁氧体烧结特性、微观结构及电磁性能的影响，首次发现了掺杂Mn离子的NiZn铁氧体其电磁性能对烧结温度具有敏感性。其次研究了不同助熔剂Bi_2O_3、WO_3和Nb_2O_5对NiCuZn铁氧体烧结特性、微观结构及电磁性能的影响，实验揭示W~(6+)离子对材料微观结构的改善；最后对低温NiCuZn铁氧体进行改性掺杂，研究稀土氧化物CeO_2对其微观结构及电磁性能的影响，并给出NiCuZn铁氧体掺杂稀土元素时的磁频谱及介频谱。
五、开发了一新型的基于不同低温烧结NiCuZn铁氧体与高介电常数(BaTiO_k+X)钙钛矿的具有电感、电容双性的铁电—铁磁复合材料，研究了不同铁电—铁磁含量对各组复合材料微观结构及电容电感双性的影响。并研究了不同助熔剂Bi_2O_3、WO_3和Nb_2O_5对其烧结特性、微观结构及电容电感双性的影响。最后对复合材料进行稀土掺杂改性，研究稀土氧化物CeO_2对其微观结构及电容电感双性的影响。
六、设计并制作出两种使用第六章LTCC复合双性材料的3G通讯设备用带通滤波器，采用Ansoft HFSS电磁仿真软件对所建立的滤波器模型进行模拟仿真，通过调节滤波器结构参数使滤波器各性能指标达到目标要求，并实现生产制备。制得带通中心频率3.5GHz，插损＜2.8dB，带宽＞400MHz，阻带衰减大于35dB的微带式带通滤波器和带通中心频率1.4GHz，插损＜3dB，带宽＞160MHz，阻带衰减大于30dB的LC式带通滤波器。
New electronic systems fo automotive/industrial/medical/aerospace will continue to challenge both packaging engineers and technology due to the increased performance requirements, higher densities, higher temperatives and limited space available. This challenge mandates the use of unique packaging techniques such as Low Temperature Co-fired Ceramic (LTCC) technology that must not only provide the increase circuit density but also the reliability, electrical and medical performance, thermal management, and hermeticity.
Low Temperature Co-fired Ceramic (LTCC) technology is a new packaging technology for integrate circuit, which consists of buried passive devices such as transformer, conductors, resistors, and capacitors in the multilayer of module and can easily integrate with active devices such as power MOS, transistors, and IC module. Recently, this technology was widely focused and researched for its wonderful properties.
Focused on the LTCC materials, we carried through some researches as follows:
1. A low temperature sintering model was established based on the liquid sintering theories. The sintering temperature and sintering time dependence of relative density for the sintered ceramics were simulated.
2. With the systemically analyses of the synthesis of ferroelectric-ferromagnetic composite materials, the low temperature sintered NiCuZn ferrites and perovskite BaTiO_k+X was chosen as the main components. A model was given by assuming the isolation of magnetic grains by surrounding non-magnetic layer to evaluate the internal field and the complex permeability of whole material as a function of the ratio of perovskite content to ferrite content.
3. We researched the effects of preparation process on the microstructure and electromagnetic properties of ceramics. The pre-sintering temperature, milling time, firing rate, sintering temperature, and holding time are changed regularly to investigate the variation of the phase formation by X-ray diffraction studies, the micrographs of the sintered ceramics by SEM, and the bulk density by Archimedes method. The frequency dependence of complex permeability, quality factor, and dielectric constant are studied.
4. The effects of sintering temperature and Mn ions contents on the microstructure and electromagnetic properties of NiZn ferrites are studied. To decreased the sintering temperature, CuO was introduced in NiZn ferrites first, and then the flux oxides such as Bi_2O_3, WO_3, and Nb_2O_5 are introduced in NiCuZn ferrites.
The variation of microstructure and electromagnetic properties with these reducing-sintering-temperature oxides' content are investigated. Finally, we researched the influence of rare earth ions Ce~(4+) on low temperature sintered NiCuZn ferrites.
5. A new ferroelectric-ferromagnetic composite material is synthesized by usual ceramic technology with NiCuZn ferrites and perovskite BaTiO_k+X as the main components. The microstructure and electromagnetic properties of the composite with different composition of NiCuZn ferrites and different perovskite contents are investigated. After that, the influences of flux oxide Bi_2O_3, WO_3, and Nb_2O_5 and the Ca~(2+), Ce~(4+) ions on this composite material are also studied.
6. A LTCC band pass filter is designed with this composite material using the Ansoft HFSS software. This filter has insertion loss in the pass band < -2.8dB, the attenuation losses in the stopband were more than 40 dB, the centre frequency of the pass band is 1.9GHz and the 3 dB band width is more than 200MHz.
引文
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