BNT微波介质陶瓷制备、低温烧结及电性能的研究
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摘要
随着微波技术的发展,微波介质陶瓷谐振器、滤波器等在卫星电视、移动通讯、雷达、电子计算机以及现代医学等众多领域中都有着广泛的应用,因此对于微波介质陶瓷的研究引起了人们极大的兴趣。本论文研究了钨青铜结构高性能微波介质陶瓷(Ba6-3xNd8+2xTi18O54(x=2/3),BNT)的粉体制备工艺、低温烧结特性及其介电性能。
BNT陶瓷固有烧结温度很高,达到1350oC,本文分别通过固相法和柠檬酸盐法制备BNT陶瓷粉体,并结合掺杂低温烧结助剂CuO-B2O3,和低熔点玻璃陶瓷粉CaO-B2O3-SiO2,研究了不同粉体制备工艺和不同掺杂剂对BNT陶瓷性能的影响。与固相法相比,使用柠檬酸盐法有利于BNT陶瓷原料在较低温度条件下析出主晶相,并可在较低的温度下烧结;掺杂不同的烧结助剂可以在低温下形成液相或玻璃相促进烧结,降低烧结温度。下面列出本次研究是主要结果:
通过固相法合成BNT陶瓷粉体后掺杂不同含量CuO-B2O3可以使BNT微波介质陶瓷在950oC致密烧结,得到的最好微波介电性能为:εr=63,Q·f=5000GHz。通过运用柠檬酸盐法制备BNT陶瓷粉体、掺杂5wt%CuO-B2O3作为烧结助剂时,可以使BNT陶瓷的烧结温度降低到925oC,此时陶瓷的εr=63,Q·f=5300GHz。为有效降低BNT陶瓷的烧结温度同时维持较好的电学性能,在BNT陶瓷中引入CaO-B2O3-SiO2微晶玻璃作为烧结助剂。CaO-B2O3-SiO2在烧结后期会部分析晶成为陶瓷相,在降低了BNT陶瓷烧结温度的同时减少了对介电性能劣化的影响,添加2wt%CaO-B2O3-SiO2的BNT陶瓷在950oC时具有更为优良的介电性能:εr=68,Q·f=7400GHz。
With the development of microwave technology, dielectric resonators and filters with excellent properties which were made up of microwave dielectric ceramics are widely used in many fields, such as satellite communications, mobile phone, modern medicine, and so on. Thereby the study of microwave dielectric ceramic materials has abstracted much attention. The fundamental purpose of this thesis is to investigate the preparation technology, low temperature sintering behavior and microwave dielectric properties of Ba6-3xNd8+2xTi18O54(x=2/3,BNT) ceramics with tungsten bornze-type structure.
BNT ceramics have a sintering temperature as high as 1350oC. The effects of different sintering aids and different preparation technologies on the electrical properties were investigated. The mixtures of CuO-B2O3 and CaO-B2O3-SiO2 were the main additives used as sintering aids. Both solid-state method and citrate sol-gel route were used for preparing ceramic powders. The principal experimental results can be concluded as follows:
Firstly, BNT ceramics were prepared by conventional solid-state method. The XRD results show that BNT ceramics have tungsten bornze-type like structure. When using CuO-B2O3 as sintering aids, it can be seen that CuO-B2O3 co-doping has an effect on the densification behavior, microstructure and microwave dielectric properties of BNT ceramics. When the content of CuO-B2O3 is 3wt%, the BNT ceramics can be well sintered at 950 oC and exhibit the best densification behavior and microwave dielectirc properties as:εr=63,Q·f=5000GHz. Secondly, a combination of chemical route derived pure powders plus the addition of a small amount of sintering aids, CuO and B2O3 was employed to decrease the sintering temperature. For 5wt% CuO-B2O3 modified BNT samples, the overall properties ofεr=63, Q·f=5300GHz and sintering temperature 925 oC are acceptable for applications. At last, the CaO-B2O3-SiO2 glass-ceramic was added into the BNT ceramic as sintering aids for not only reducing the sintering temperature but keeping the microwave dielectric properties at a high level as well. CaO-B2O3-SiO2 glass-ceramic has a low melting temperature and some of them were crystallized to form ceramic phase after sintering. With 2wt% content of CaO-B2O3-SiO2, the BNT ceramics can be well sintered at 950oC and show a good microwave dielectric properties asεr=68,Q·f=7400GHz.
BNT陶瓷固有烧结温度很高,达到1350oC,本文分别通过固相法和柠檬酸盐法制备BNT陶瓷粉体,并结合掺杂低温烧结助剂CuO-B2O3,和低熔点玻璃陶瓷粉CaO-B2O3-SiO2,研究了不同粉体制备工艺和不同掺杂剂对BNT陶瓷性能的影响。与固相法相比,使用柠檬酸盐法有利于BNT陶瓷原料在较低温度条件下析出主晶相,并可在较低的温度下烧结;掺杂不同的烧结助剂可以在低温下形成液相或玻璃相促进烧结,降低烧结温度。下面列出本次研究是主要结果:
通过固相法合成BNT陶瓷粉体后掺杂不同含量CuO-B2O3可以使BNT微波介质陶瓷在950oC致密烧结,得到的最好微波介电性能为:εr=63,Q·f=5000GHz。通过运用柠檬酸盐法制备BNT陶瓷粉体、掺杂5wt%CuO-B2O3作为烧结助剂时,可以使BNT陶瓷的烧结温度降低到925oC,此时陶瓷的εr=63,Q·f=5300GHz。为有效降低BNT陶瓷的烧结温度同时维持较好的电学性能,在BNT陶瓷中引入CaO-B2O3-SiO2微晶玻璃作为烧结助剂。CaO-B2O3-SiO2在烧结后期会部分析晶成为陶瓷相,在降低了BNT陶瓷烧结温度的同时减少了对介电性能劣化的影响,添加2wt%CaO-B2O3-SiO2的BNT陶瓷在950oC时具有更为优良的介电性能:εr=68,Q·f=7400GHz。
With the development of microwave technology, dielectric resonators and filters with excellent properties which were made up of microwave dielectric ceramics are widely used in many fields, such as satellite communications, mobile phone, modern medicine, and so on. Thereby the study of microwave dielectric ceramic materials has abstracted much attention. The fundamental purpose of this thesis is to investigate the preparation technology, low temperature sintering behavior and microwave dielectric properties of Ba6-3xNd8+2xTi18O54(x=2/3,BNT) ceramics with tungsten bornze-type structure.
BNT ceramics have a sintering temperature as high as 1350oC. The effects of different sintering aids and different preparation technologies on the electrical properties were investigated. The mixtures of CuO-B2O3 and CaO-B2O3-SiO2 were the main additives used as sintering aids. Both solid-state method and citrate sol-gel route were used for preparing ceramic powders. The principal experimental results can be concluded as follows:
Firstly, BNT ceramics were prepared by conventional solid-state method. The XRD results show that BNT ceramics have tungsten bornze-type like structure. When using CuO-B2O3 as sintering aids, it can be seen that CuO-B2O3 co-doping has an effect on the densification behavior, microstructure and microwave dielectric properties of BNT ceramics. When the content of CuO-B2O3 is 3wt%, the BNT ceramics can be well sintered at 950 oC and exhibit the best densification behavior and microwave dielectirc properties as:εr=63,Q·f=5000GHz. Secondly, a combination of chemical route derived pure powders plus the addition of a small amount of sintering aids, CuO and B2O3 was employed to decrease the sintering temperature. For 5wt% CuO-B2O3 modified BNT samples, the overall properties ofεr=63, Q·f=5300GHz and sintering temperature 925 oC are acceptable for applications. At last, the CaO-B2O3-SiO2 glass-ceramic was added into the BNT ceramic as sintering aids for not only reducing the sintering temperature but keeping the microwave dielectric properties at a high level as well. CaO-B2O3-SiO2 glass-ceramic has a low melting temperature and some of them were crystallized to form ceramic phase after sintering. With 2wt% content of CaO-B2O3-SiO2, the BNT ceramics can be well sintered at 950oC and show a good microwave dielectric properties asεr=68,Q·f=7400GHz.
引文
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