PTC陶瓷的细晶化及其与Ni电极共烧技术研究
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摘要
为适应电子元器件的小型化、片式化、高性能的发展需要,PTCR也必须朝着小型、多层片式化的方向发展。PTC半导瓷是利用晶界效应的功能陶瓷,要获取高性能的多层片式PTC瓷,必须使多层片式PTCR单层瓷体在垂直电极方向上包含一定数量的晶界,而多层片式PTCR单层瓷体的厚度只有10-40μm,这就要求晶粒尺寸随之相应的减小,至少使单层PTC瓷体具有一定数量的晶界,因而晶粒尺寸应该在0.5-2μm。本文以制取高性能片式PTC陶瓷为目标,对水热法和固相法的BaTiO3基细晶PTC瓷的制备、高性能Ni内电极浆料的制备及与瓷体匹配问题、细晶PTC陶瓷流延工艺优化、界面效应与气氛对片式PTC陶瓷性能影响、再氧化处理与片式PTC陶瓷性能的关系等展开研究工作。
本文以水热法粉体和固相法粉体为原料,通过适当提高施受主掺杂比、提高预烧温度、降低烧结温度、添加不同玻璃相等方法来减小陶瓷的晶粒尺寸和改善PTC电学性能。采用市售水热法粉体作为原料制备了平均晶粒尺寸为2-5μm、室温电阻率在100Ω·cm左右、升阻比大于104的半导化良好圆片型PTC,实验表明水热法粉体存在钡钛比失衡、杂质多等缺点使进一步减小晶粒尺寸存在极限；而采用传统固相法粉体作为原料,通过调整Y/Mn、经1220℃预烧和1300℃烧结等方法得到平均晶粒尺寸2μm、室温电阻率为205Ω·cm、升阻比大于104的圆片型PTC。
多层片式PTCR用Ni内电极制作过程中,为获取性能良好的Ni内电极浆料,Ni粉为采用的液相还原法制备的亚微米级粉体,有机溶剂选用松油醇和邻苯二甲酸二丁酯,有机粘合剂选用松香,Ni电极浆料中BaTiO3粉的添加量为10wt%,促使电极与陶瓷线胀系数趋于一致,很好的解决了分层现象的发生,Ni电极中还加入了15wt%Cr粉,提高了电极的抗氧化温度、同时在后续再氧化处理过程中起到很好保护Ni电极的作用。
而采用固相法粉料的有机流延法,通过适当增加施受主掺杂比、提高预烧温度,降低烧结温度等方法来实现了陶瓷晶粒尺寸的细小化和PTC性能的优越化；适当提高流延浆料固含量后实验表明PTC具有更好的升阻比、更小的晶粒尺寸、更低的室温电阻率,通过A位引入Ca和Sr结合高能球磨的方法,空气中烧结制备出了晶粒尺寸为1.5μm、室温电阻率为150Ω·cm、密度为5.64g／cm3、升阻比达4.5数量级的的PTC陶瓷。
本文最后研究了片式PTC陶瓷的还原烧结机制、再氧化机制与叠层体性能之间关系、Ni-BaTiO3界面效应与多层片式PTCR性能关系。片式PTC陶瓷在N2/H2混合气氛内于1240-1320℃烧结0.5小时,其中氧分压PO2=10-8-10-12MPa,在1050-1280℃以400℃/h升温速率,高温降到850℃选定的降温速率为300℃/h,温度降到850℃时,停止通气直到室温。800℃其再氧化1h,片式PTC陶瓷晶粒尺寸小于1μm、升阻比为2.5个数量级、室温电阻率为98.8Ω·cm。界面效应实验表明适度的金属-陶瓷互扩散对形成性能优异的多层片式PTCR很有好处,但是过重的互扩散会恶化多层片式PTCR的性能。瓷体与Ni电极的共烧中的扩散等效应为多层片式PTCR的研制奠定了一定的实验基础。
In order to meet the miniaturization of electronic components, chip-based, high-performance development needs, PTCR must also be moving in a small, multi-chip-oriented direction. To obtain high-performance multi-layer chip PTCR as much as possible, We must make multi-layer chip PTCR body in the vertical direction contains a number of grain, while the multi-layer chip PTCR body thickness of single-layer is 10-40μm, which requires the corresponding reduction in grain size. The single-layer must at least include many grain boundaries, so the grain size should be between 0.5μm and 2μm. Preparation of this paper, high-performance multi-layer chip PTCR was the target, hydrothermal method and solid-phase method of fine-grained BaTiO3-based PTC ceramics were used, which high-performance nickel electrodes and the matching issue of electrode and ceramic, the best tape casting process to obtain fine-grained ceramic, interface effects and atmosphere on the PTCR properties of multilayer chip relations, the relationship between re-oxidation method and the properties of multi-layer chip PTCR were researched.
In this paper, powder by hydrothermal method and solid-phase powder as raw material, through improving the ratio of acceptor and dopant, improving pre-sintering temperature, decreasing sintering temperature, adding the equivalent of different ways, we reduced the glass-ceramic grain size and improved the electrical properties of PTC. By hydrothermal method using outsourcing as a raw material powder we got the PTCR with an average grain size of 2-5μm, room-temperature resistivity in the 100Ω·cm or so, lift-drag ratio greater than 104, but the hydrothermal method presence of barium titanium powder ratio imbalanced, impurities and other defects was difficult to further reduce its grain size; using the traditional solid-phase powder as raw material, by adjusting the Y/Mn, after pre-sintering at 1220℃,sintering at 1300℃including other methods we got the PTC with an average of grain size of 2μm, room-temperature resistivity of 205Ω·cm, lift-drag ratio greater than 104.
Within the process of Ni inner electrode production for multilayer chip PTCR, in order to obtain good performance Ni electrode paste, sub-micron Ni powder was gotten by liquid-phase reduction method. Alcohol and pine oil phthalate ding ester were used for organic solvent, rosin was selected for organic binder. Ni electrode paste in the adding amount of 10 wt% BaTiO3 powder could promote a better match between electrode and ceramic, which was a good solution to the occurrence of stratification. The 15 wt% Cr powder was also joined in Ni electrode, adjusting the sintering temperature of electrode, increasing the use temperature of electrode which played the well-protected role of Ni electrode in re-oxidation process.
We used the method of organic cast of which powders were gotten by solid-phase, through increasing the ratio of acceptor and doping appropriately, increasing the pre-sintering temperature, lowering sintering temperature and other methods we achieve a small grain size of ceramic which had good performance. By improving the solids extension of flow slurry, experiments showed that the PTC had a better lift-drag ratio, smaller grain size, lower electrical resistivity at room temperature. Through introducing Ca used for the A-bit diversified and using the method of high-energy ball milling we obtained the PTC of which grain size was 1.5μm, room-temperature resistivity was 150Ω·cm, density was 5.64 g/cm3, lift-drag ratio was up to 4.5 orders of magnitude.
We studied the mechanism of the multilayer chip PTCR in the sintering surrounding of reducing oxygen, with the relationship between re-oxidation mechanism and the the performance of laminated body, the relationship between Ni-BaTiO3 interface effect and multi-layer chip PTCR properties were also researched. The green sheets with Ni paste as inner electrodes were sintered at 1240-1320℃for half an hour under a N2/H2 mixing gas with the oxygen partial pressure P(O2)=10-8-10-12 MPa, and then re-oxidation at 800℃for one hour to form multilayer PTCR. In the process of 1050-1280℃and high temperature down to 850℃, the heating rate and cooling rate were 400℃/h and 300℃/h. With this mechanism we got we got the PTC with an average of grain size of less than 1μm, room-temperature resistivity of 98.8Ω·cm, lift-drag ratio of 2.5 orders of magnitude. Interface effect experiments showed that an appropriate degree of metal-ceramic inter-diffusion on the formation of high performance multi-layer chip PTCR was very good, but too heavy inter-diffusion could worse the performance of multi-layer chip PTCR. Dispersion effects in ceramics cofired with Ni electrodes were benefit for the development of multilayer chip PTCR.
本文以水热法粉体和固相法粉体为原料,通过适当提高施受主掺杂比、提高预烧温度、降低烧结温度、添加不同玻璃相等方法来减小陶瓷的晶粒尺寸和改善PTC电学性能。采用市售水热法粉体作为原料制备了平均晶粒尺寸为2-5μm、室温电阻率在100Ω·cm左右、升阻比大于104的半导化良好圆片型PTC,实验表明水热法粉体存在钡钛比失衡、杂质多等缺点使进一步减小晶粒尺寸存在极限；而采用传统固相法粉体作为原料,通过调整Y/Mn、经1220℃预烧和1300℃烧结等方法得到平均晶粒尺寸2μm、室温电阻率为205Ω·cm、升阻比大于104的圆片型PTC。
多层片式PTCR用Ni内电极制作过程中,为获取性能良好的Ni内电极浆料,Ni粉为采用的液相还原法制备的亚微米级粉体,有机溶剂选用松油醇和邻苯二甲酸二丁酯,有机粘合剂选用松香,Ni电极浆料中BaTiO3粉的添加量为10wt%,促使电极与陶瓷线胀系数趋于一致,很好的解决了分层现象的发生,Ni电极中还加入了15wt%Cr粉,提高了电极的抗氧化温度、同时在后续再氧化处理过程中起到很好保护Ni电极的作用。
而采用固相法粉料的有机流延法,通过适当增加施受主掺杂比、提高预烧温度,降低烧结温度等方法来实现了陶瓷晶粒尺寸的细小化和PTC性能的优越化；适当提高流延浆料固含量后实验表明PTC具有更好的升阻比、更小的晶粒尺寸、更低的室温电阻率,通过A位引入Ca和Sr结合高能球磨的方法,空气中烧结制备出了晶粒尺寸为1.5μm、室温电阻率为150Ω·cm、密度为5.64g／cm3、升阻比达4.5数量级的的PTC陶瓷。
本文最后研究了片式PTC陶瓷的还原烧结机制、再氧化机制与叠层体性能之间关系、Ni-BaTiO3界面效应与多层片式PTCR性能关系。片式PTC陶瓷在N2/H2混合气氛内于1240-1320℃烧结0.5小时,其中氧分压PO2=10-8-10-12MPa,在1050-1280℃以400℃/h升温速率,高温降到850℃选定的降温速率为300℃/h,温度降到850℃时,停止通气直到室温。800℃其再氧化1h,片式PTC陶瓷晶粒尺寸小于1μm、升阻比为2.5个数量级、室温电阻率为98.8Ω·cm。界面效应实验表明适度的金属-陶瓷互扩散对形成性能优异的多层片式PTCR很有好处,但是过重的互扩散会恶化多层片式PTCR的性能。瓷体与Ni电极的共烧中的扩散等效应为多层片式PTCR的研制奠定了一定的实验基础。
In order to meet the miniaturization of electronic components, chip-based, high-performance development needs, PTCR must also be moving in a small, multi-chip-oriented direction. To obtain high-performance multi-layer chip PTCR as much as possible, We must make multi-layer chip PTCR body in the vertical direction contains a number of grain, while the multi-layer chip PTCR body thickness of single-layer is 10-40μm, which requires the corresponding reduction in grain size. The single-layer must at least include many grain boundaries, so the grain size should be between 0.5μm and 2μm. Preparation of this paper, high-performance multi-layer chip PTCR was the target, hydrothermal method and solid-phase method of fine-grained BaTiO3-based PTC ceramics were used, which high-performance nickel electrodes and the matching issue of electrode and ceramic, the best tape casting process to obtain fine-grained ceramic, interface effects and atmosphere on the PTCR properties of multilayer chip relations, the relationship between re-oxidation method and the properties of multi-layer chip PTCR were researched.
In this paper, powder by hydrothermal method and solid-phase powder as raw material, through improving the ratio of acceptor and dopant, improving pre-sintering temperature, decreasing sintering temperature, adding the equivalent of different ways, we reduced the glass-ceramic grain size and improved the electrical properties of PTC. By hydrothermal method using outsourcing as a raw material powder we got the PTCR with an average grain size of 2-5μm, room-temperature resistivity in the 100Ω·cm or so, lift-drag ratio greater than 104, but the hydrothermal method presence of barium titanium powder ratio imbalanced, impurities and other defects was difficult to further reduce its grain size; using the traditional solid-phase powder as raw material, by adjusting the Y/Mn, after pre-sintering at 1220℃,sintering at 1300℃including other methods we got the PTC with an average of grain size of 2μm, room-temperature resistivity of 205Ω·cm, lift-drag ratio greater than 104.
Within the process of Ni inner electrode production for multilayer chip PTCR, in order to obtain good performance Ni electrode paste, sub-micron Ni powder was gotten by liquid-phase reduction method. Alcohol and pine oil phthalate ding ester were used for organic solvent, rosin was selected for organic binder. Ni electrode paste in the adding amount of 10 wt% BaTiO3 powder could promote a better match between electrode and ceramic, which was a good solution to the occurrence of stratification. The 15 wt% Cr powder was also joined in Ni electrode, adjusting the sintering temperature of electrode, increasing the use temperature of electrode which played the well-protected role of Ni electrode in re-oxidation process.
We used the method of organic cast of which powders were gotten by solid-phase, through increasing the ratio of acceptor and doping appropriately, increasing the pre-sintering temperature, lowering sintering temperature and other methods we achieve a small grain size of ceramic which had good performance. By improving the solids extension of flow slurry, experiments showed that the PTC had a better lift-drag ratio, smaller grain size, lower electrical resistivity at room temperature. Through introducing Ca used for the A-bit diversified and using the method of high-energy ball milling we obtained the PTC of which grain size was 1.5μm, room-temperature resistivity was 150Ω·cm, density was 5.64 g/cm3, lift-drag ratio was up to 4.5 orders of magnitude.
We studied the mechanism of the multilayer chip PTCR in the sintering surrounding of reducing oxygen, with the relationship between re-oxidation mechanism and the the performance of laminated body, the relationship between Ni-BaTiO3 interface effect and multi-layer chip PTCR properties were also researched. The green sheets with Ni paste as inner electrodes were sintered at 1240-1320℃for half an hour under a N2/H2 mixing gas with the oxygen partial pressure P(O2)=10-8-10-12 MPa, and then re-oxidation at 800℃for one hour to form multilayer PTCR. In the process of 1050-1280℃and high temperature down to 850℃, the heating rate and cooling rate were 400℃/h and 300℃/h. With this mechanism we got we got the PTC with an average of grain size of less than 1μm, room-temperature resistivity of 98.8Ω·cm, lift-drag ratio of 2.5 orders of magnitude. Interface effect experiments showed that an appropriate degree of metal-ceramic inter-diffusion on the formation of high performance multi-layer chip PTCR was very good, but too heavy inter-diffusion could worse the performance of multi-layer chip PTCR. Dispersion effects in ceramics cofired with Ni electrodes were benefit for the development of multilayer chip PTCR.
引文
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