低阻Ni/（Ba，Sr）TiO_3复合PTC材料的制备与电性能研究
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摘要
为了研制具备良好PTC性能的低阻材料,对(Ba,Sr)TiO_3陶瓷以及Ni/(Ba,Sr)TiO_3复合材料进行了研究。采用了ESEM、OG、TEM、EDX、SAD、XRD、XPS、DSC-TG等现代材料研究与分析方法。测试了材料的电阻-温度特性和耐电压强度。讨论了Ni/(Ba,Sr)TiO_3复合PTC材料的性能特点和影响因素。
通过增加MnO_2添加量、添加BN、加入Zn-V-B系玻璃料以及改变预合成所用的TiO_2原料四种途径来改善(Ba,Sr)TiO_3陶瓷的PTC性能。这四种途径在增强PTC效应方面均起到了积极的效果。尤其是不改变配方,采用TiO_2-B原料制备出的(Ba,Sr)TiO_3陶瓷材料PTC性能最为理想。1320℃保温20min烧结后,ρ_(25) = 228.9Ω·cm,ρ_(max)/ρ25=10~(5.1),α= 25.1%/℃。采用此配方和原料制备与金属Ni复合的陶瓷基质。在还原气氛中烧成后,随着Ni加入量增大,Ni/(Ba,Sr)TiO_3复合材料室温电阻率降低,同时PTC效应恶化、耐电压强度下降。综合考虑各项电性能指标,下面研究中将Ni的加入量固定在15wt%。提高烧结温度,有助于制备高性能的Ni/(Ba,Sr)TiO_3复合PTC材料。对比了复合材料在倒置的Al2O_3坩埚内放置足够多石墨粉形成的还原气氛1、石墨坩埚形成的还原气氛2中烧结后以及热处理后的XRD和XPS图谱,结果表明还原气氛1更适合制备复合PTC材料。另外,所采用的三种Ni粉中,Ni粉平均粒径越小,室温电阻率越小,PTC效应越好。在复合材料中引入了PbO-B_2O_3-ZnO-SiO_2玻璃料。此玻璃料可以很好地润湿(Ba,Sr)TiO_3陶瓷。玻璃料以无定形态存在于复合材料中的相界与陶瓷晶界上。晶粒间相和陶瓷之间没有明显的扩散。玻璃料的加入不仅有助于复合材料的致密化,而且有助于Ni颗粒在陶瓷基质中的均匀分布,更为重要的是可以改变Ni-(Ba,Sr)TiO_3相界面上的电荷传输,从而改善了复合材料的电性能。当玻璃料加入量为0.5wt% ,AST加入量为0.1wt%时,Ni-(Ba,Sr)TiO_3相界面上的液相层厚度适中,既可以避免金属-陶瓷界面上隧道效应对PTC效应的消弱,又不足以因为液相层过厚导致晶界电阻过大,复合材料获得了较佳的电性能。与AST相比,玻璃料更有利于制备高性能的Ni/(Ba,Sr)TiO_3复合PTC材料。仅加入0.6wt%玻璃料,Ni/(Ba,Sr)TiO_3复合材料1320℃保温20min烧结后获得了最佳的电性能(ρ25=2.5Ω·cm,ρ_(max)/ρ_(25)=10~(3.6),α= 9.0 %/℃)。计算了(Ba,Sr)TiO_3陶瓷中的有效施主浓度,肯定了Ni-(Ba,Sr)TiO_3界面上通过隧道效应实现欧姆接触的可行性。对制备高性能Ni/BaTiO_3复合PTC材料提出了改进措施,并提出了理想的显微结构模型。
In order to fabricate the material with both low room-temperature resistivity and considerable PTC effect, (Ba,Sr)TiO_3 ceramics and Ni/(Ba,Sr)TiO_3 composite were investigated. ESEM, OG, TEM, EDX, SAD, XRD, XPS as well as DSC-TG were employed to investigate the samples. Resistivity-temperature characteristics and withstanding voltage strength of the samples were obtained. The properties and the influential factors of Ni/(Ba,Sr)TiO_3 PTC composite were discussed.
Four approaches, namely, increasing MnO_2 amount, introducing BN, adding Zn-V-B glass and using another TiO_2 powder as the raw material, were used to improve the PTC effect of (Ba,Sr)TiO_3 ceramics. They all play positive effects in enhancing the PTC effect. Particularly, with the same composition and the specific TiO_2-B powder, electrical properties of (Ba,Sr)TiO_3 ceramics are excellent. Sintering at 1320℃for 20min, the room-temperature resistivity (ρ_(25)) is 228.9Ω·cm, the resistivity jump (ρ_(max)/ρ_(25)) is 10~(5.1) and the resistivity-temperature coefficient (α) is 25.1 %/oC. The (Ba,Sr)TiO_3 ceramic matrix, used in the Ni/(Ba,Sr)TiO_3 composite fabrication, was according to the specific composition and raw materials.
When a Ni/(Ba,Sr)TiO_3 composite is sintered in the reducing atmosphere,ρ25 decreases, the PTC effect worsens and the withstanding voltage strength decreases with increasing the nickel amount. Taking all the electrical parameters into consideration, nickel amount is fixed at 15wt% in the following experiment. With increasing the sintering temperature, Ni/(Ba,Sr)TiO_3 PTC composite finds better electrical properties. XRD and XPS spectrum comparison of the composite sintered in the 1st reducing atmosphere (Samples are put on an alumina setter in a bottom-up alumina crucible. Sufficient graphite powder is placed beside the samples in the crucible and there is no contact between the graphite powder and the samples), in the 2nd reducing atmosphere (produced by graphite crucible) and after the heat treatment shows that, the 1st reducing atmosphere is desirable for the fabrication of PTC composite. Particle size distribution of nickel powders also influences the electrical properties of the composite. Concerning the three nickel powders used, the smaller the average particle size, the lower theρ_(25) and the better the PTC effect.
PbO-B_2O_3-ZnO-SiO_2 glass has been introduced into the composite. Good wet behavior between the glass and (Ba,Sr)TiO_3 ceramics can be observed. The glass has an amorphous structure and exists at the composite phase interface and ceramic grain boundary. No obvious diffusion occurs at the interface between crystalline (Ba,Sr)TiO_3 grain and the intergranular phase. The addition of glass not only improves the densification process but also helps the homogeneous distribution of nickel particles in the ceramic matrix. More importantly, charge transport behavior at the Ni-(Ba,Sr)TiO_3 interface is modified by the glass addition, the electrical properties are thus improved. With 0.5wt% glass and 0.1wt% AST as the sintering aid, the electrical properties of the composite are better. It is ascribed to the proper intergranular layer, which effectively avoids electron tunneling at the metal-ceramics interface and PTC deterioration. Also the intergranular layer is thin enough not to greatly increase grain-boundary resistance. Comparing with AST, glass favors the fabrication of Ni/(Ba,Sr)TiO_3 PTC composite with high performance. When a Ni/(Ba,Sr)TiO_3 composite with only 0.6wt% glass as the sintering aid is sintered at 1320℃for 20min, the composite possesses the optimized electrical properties. The room-temperature resistivity is 2.5Ω·cm, the resistivity jump is about 103.6 and the resistivity-temperature coefficient is 9.0 %/℃.
The effective donor concentration in the (Ba,Sr)TiO_3 ceramics is calculated and the Ohmic contact via the quantum mechanical tunneling effect at the Ni-(Ba,Sr)TiO_3 interface is feasible. Improvement measures are proposed and the ideal structural model for Ni/BaTiO_3 PTC composite is sketched.
通过增加MnO_2添加量、添加BN、加入Zn-V-B系玻璃料以及改变预合成所用的TiO_2原料四种途径来改善(Ba,Sr)TiO_3陶瓷的PTC性能。这四种途径在增强PTC效应方面均起到了积极的效果。尤其是不改变配方,采用TiO_2-B原料制备出的(Ba,Sr)TiO_3陶瓷材料PTC性能最为理想。1320℃保温20min烧结后,ρ_(25) = 228.9Ω·cm,ρ_(max)/ρ25=10~(5.1),α= 25.1%/℃。采用此配方和原料制备与金属Ni复合的陶瓷基质。在还原气氛中烧成后,随着Ni加入量增大,Ni/(Ba,Sr)TiO_3复合材料室温电阻率降低,同时PTC效应恶化、耐电压强度下降。综合考虑各项电性能指标,下面研究中将Ni的加入量固定在15wt%。提高烧结温度,有助于制备高性能的Ni/(Ba,Sr)TiO_3复合PTC材料。对比了复合材料在倒置的Al2O_3坩埚内放置足够多石墨粉形成的还原气氛1、石墨坩埚形成的还原气氛2中烧结后以及热处理后的XRD和XPS图谱,结果表明还原气氛1更适合制备复合PTC材料。另外,所采用的三种Ni粉中,Ni粉平均粒径越小,室温电阻率越小,PTC效应越好。在复合材料中引入了PbO-B_2O_3-ZnO-SiO_2玻璃料。此玻璃料可以很好地润湿(Ba,Sr)TiO_3陶瓷。玻璃料以无定形态存在于复合材料中的相界与陶瓷晶界上。晶粒间相和陶瓷之间没有明显的扩散。玻璃料的加入不仅有助于复合材料的致密化,而且有助于Ni颗粒在陶瓷基质中的均匀分布,更为重要的是可以改变Ni-(Ba,Sr)TiO_3相界面上的电荷传输,从而改善了复合材料的电性能。当玻璃料加入量为0.5wt% ,AST加入量为0.1wt%时,Ni-(Ba,Sr)TiO_3相界面上的液相层厚度适中,既可以避免金属-陶瓷界面上隧道效应对PTC效应的消弱,又不足以因为液相层过厚导致晶界电阻过大,复合材料获得了较佳的电性能。与AST相比,玻璃料更有利于制备高性能的Ni/(Ba,Sr)TiO_3复合PTC材料。仅加入0.6wt%玻璃料,Ni/(Ba,Sr)TiO_3复合材料1320℃保温20min烧结后获得了最佳的电性能(ρ25=2.5Ω·cm,ρ_(max)/ρ_(25)=10~(3.6),α= 9.0 %/℃)。计算了(Ba,Sr)TiO_3陶瓷中的有效施主浓度,肯定了Ni-(Ba,Sr)TiO_3界面上通过隧道效应实现欧姆接触的可行性。对制备高性能Ni/BaTiO_3复合PTC材料提出了改进措施,并提出了理想的显微结构模型。
In order to fabricate the material with both low room-temperature resistivity and considerable PTC effect, (Ba,Sr)TiO_3 ceramics and Ni/(Ba,Sr)TiO_3 composite were investigated. ESEM, OG, TEM, EDX, SAD, XRD, XPS as well as DSC-TG were employed to investigate the samples. Resistivity-temperature characteristics and withstanding voltage strength of the samples were obtained. The properties and the influential factors of Ni/(Ba,Sr)TiO_3 PTC composite were discussed.
Four approaches, namely, increasing MnO_2 amount, introducing BN, adding Zn-V-B glass and using another TiO_2 powder as the raw material, were used to improve the PTC effect of (Ba,Sr)TiO_3 ceramics. They all play positive effects in enhancing the PTC effect. Particularly, with the same composition and the specific TiO_2-B powder, electrical properties of (Ba,Sr)TiO_3 ceramics are excellent. Sintering at 1320℃for 20min, the room-temperature resistivity (ρ_(25)) is 228.9Ω·cm, the resistivity jump (ρ_(max)/ρ_(25)) is 10~(5.1) and the resistivity-temperature coefficient (α) is 25.1 %/oC. The (Ba,Sr)TiO_3 ceramic matrix, used in the Ni/(Ba,Sr)TiO_3 composite fabrication, was according to the specific composition and raw materials.
When a Ni/(Ba,Sr)TiO_3 composite is sintered in the reducing atmosphere,ρ25 decreases, the PTC effect worsens and the withstanding voltage strength decreases with increasing the nickel amount. Taking all the electrical parameters into consideration, nickel amount is fixed at 15wt% in the following experiment. With increasing the sintering temperature, Ni/(Ba,Sr)TiO_3 PTC composite finds better electrical properties. XRD and XPS spectrum comparison of the composite sintered in the 1st reducing atmosphere (Samples are put on an alumina setter in a bottom-up alumina crucible. Sufficient graphite powder is placed beside the samples in the crucible and there is no contact between the graphite powder and the samples), in the 2nd reducing atmosphere (produced by graphite crucible) and after the heat treatment shows that, the 1st reducing atmosphere is desirable for the fabrication of PTC composite. Particle size distribution of nickel powders also influences the electrical properties of the composite. Concerning the three nickel powders used, the smaller the average particle size, the lower theρ_(25) and the better the PTC effect.
PbO-B_2O_3-ZnO-SiO_2 glass has been introduced into the composite. Good wet behavior between the glass and (Ba,Sr)TiO_3 ceramics can be observed. The glass has an amorphous structure and exists at the composite phase interface and ceramic grain boundary. No obvious diffusion occurs at the interface between crystalline (Ba,Sr)TiO_3 grain and the intergranular phase. The addition of glass not only improves the densification process but also helps the homogeneous distribution of nickel particles in the ceramic matrix. More importantly, charge transport behavior at the Ni-(Ba,Sr)TiO_3 interface is modified by the glass addition, the electrical properties are thus improved. With 0.5wt% glass and 0.1wt% AST as the sintering aid, the electrical properties of the composite are better. It is ascribed to the proper intergranular layer, which effectively avoids electron tunneling at the metal-ceramics interface and PTC deterioration. Also the intergranular layer is thin enough not to greatly increase grain-boundary resistance. Comparing with AST, glass favors the fabrication of Ni/(Ba,Sr)TiO_3 PTC composite with high performance. When a Ni/(Ba,Sr)TiO_3 composite with only 0.6wt% glass as the sintering aid is sintered at 1320℃for 20min, the composite possesses the optimized electrical properties. The room-temperature resistivity is 2.5Ω·cm, the resistivity jump is about 103.6 and the resistivity-temperature coefficient is 9.0 %/℃.
The effective donor concentration in the (Ba,Sr)TiO_3 ceramics is calculated and the Ohmic contact via the quantum mechanical tunneling effect at the Ni-(Ba,Sr)TiO_3 interface is feasible. Improvement measures are proposed and the ideal structural model for Ni/BaTiO_3 PTC composite is sketched.
引文
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