块体、厚膜和薄膜NTC热敏电阻的制备与性能
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摘要
具有AB_2O_4尖晶石结构的Mn系过渡金属氧化物是NTC热敏电阻主要的材料体系；高性能膜状(厚膜和薄膜)NTC热敏电阻的制备是NTC热敏电阻领域的研究热点；多晶膜状NTC热敏电阻的导电机理研究是目前热敏电阻理论研究中的难点与重点。
本文选择Mn系尖晶石NTC体系为主要研究对象；以实现NTC热敏电阻的膜状化和解决多晶膜状NTC热敏电阻导电机理中的难点为主要研究目标；在大量块体NTC热敏电阻的实验数据为基础上，以丝网印刷法制备厚膜NTC热敏电阻、溶胶-凝胶法制备薄膜NTC热敏电阻和变温复阻抗谱分析多晶膜状NTC热敏电阻的导电机理为主要技术途径，开展了一系列的研究工作。对块体、厚膜和薄膜NTC热敏电阻的制备工艺参数进行了较系统的研究；以小极化子跳跃导电理论为基础，采用复阻抗谱的方法分析了影响厚膜和薄膜NTC热敏电阻性能的主要工艺参数对其导电机理的影响。
首先，研究了组分、烧结温度和粉体制备方法对Mn-Ni-O二元系、Mn-Co-Ni-O三元系和Mn-Co-Ni-Cu-O四元系块体热敏电阻的微结构和电性能的影响，结果表明：采用溶胶-凝胶法合成的粉体，烧结温度为1180oC，保温时间为3h，组分为Ni_(0.85)Co_(0.3)Mn_(1.85)O_4(MCN)的块体热敏电阻各项性能均较优异。
其次，基于块体NTC热敏电阻实验数据，采用丝网印刷法在Al_2O_3基底上制备了MCN厚膜热敏电阻，讨论了固含量(50%、67%和75%)、烧结温度(1150、1180和1200oC)和电极形状(端电极和叉指电极)对MCN厚膜热敏电阻微结构和电性能的影响。结果表明：固含量为67%，烧结温度为1180oC时，制备有端电极和叉指电极的MCN厚膜热敏电阻的性能均较优异。采用端电极的MCN厚膜R-T关系满足指数关系(R=R0exp(B/T))，而采用叉指电极的厚膜热敏电阻的R-T关系为线性关系(R=R0+AT)。分析了电极形状对MCN厚膜热敏电阻R-T关系的影响：端电极MCN厚膜热敏电阻，端电极的宽度并不会影响其R-T关系的指数关系；叉指电极MCN厚膜热敏电阻，叉指间距离的改变不会影响其R-T关系的线性关系；叉指长度(a值)的大小是影响其R-T关系的主要原因；当a值变小时，厚膜热敏电阻的R-T关系由开始的线性关系慢慢过渡到指数关系。采用Ansoft maxwell12软件对MCN厚膜的电势能和电场分布进行了简单的分析。
第三，采用溶胶-凝胶法在Al_2O_3基底上成功制备了MCN薄膜热敏电阻。研究了退火温度(650、700、750和800°C)和薄膜厚度(519.6、627.8和742.3nm)对MCN薄膜微结构和电性能的影响。对于MCN薄膜热敏电阻而言，750°C为最佳的退火温度。750°C下制备的MCN薄膜热敏电阻的室温电阻R_(25)=4.8MΩ，特征温度T_0=3720.6K，老化系数ΔR/R=3.7%。厚度对MCN薄膜热敏电阻的T_0值影响不大；样品R_(25)随着厚度的增加而减小，近似于线性减小；厚度对MCN薄膜热敏电阻的老化系数影响不大。为了达到减小电阻值的目的，采用溶胶-凝胶法在Al_2O_3基底上，700°C退火温度下，成功制备了Ni_(0.85)Co_(0.3)CuxMn_(1.85-x)O_4(MCCN，x=0，0.15，0.3和0.45)薄膜，研究了组分对MCCN薄膜热敏电阻的微观结构和电性能的影响。对于MCCN薄膜热敏电阻而言，当x=0.15，MCCN热敏电阻的R_(25)较小(0.56MΩ)，灵敏度较高(T_0=4107.0K)，老化系数较小(ΔR/R=5.7%)，为较合适的组分。
第四，通过对具有不同叉指长度(a值)的叉指电极MCN厚膜热敏电阻的变温复阻抗谱的分析，我们得到了具有不同a值的MCN厚膜热敏电阻中晶粒与晶界的R-T特性。样品中晶界电阻(R_(gb))均大于晶粒电阻(R_g)；晶粒内部电子的输运为变程跳跃(VRH)；a值越大，晶粒电阻和特征温度越小；当a值变小时，样品晶界的R_(gb)-T关系由开始的线性关系慢慢过渡到指数关系，这是引起厚膜热敏电阻R-T关系随a值大小发生变化的主要原因。
第五，通过对不同晶粒尺寸的MCN薄膜热敏电阻变温复阻抗谱的分析，我们得到了：在不同晶粒尺寸的MCN薄膜热敏电阻中，晶粒与晶界处电子的导电均为跳跃导电； R_(gb)均大于R_g，这说明材料的电阻由晶界主导；而晶粒特征温度(T_0~g)均大于晶界特征温度(T_0gb)，这说明材料中特征温度由晶粒主导。晶界的电子跳跃形式为最近邻跳跃(NNH)，而晶粒内部电子的跳跃形式为由VRH向NNH过渡的跳跃方式，薄膜热敏电阻中电子跳跃形式为NNH主导的，VRH和NNH相结合的跳跃形式。
NTC厚膜和薄膜热敏电阻制备工艺参数的研究以及内部导电机理的分析将为NTC厚膜和薄膜的工业应用提供有意义的指导。
Manganite based transition metal oxide ceramics with AB_2O_4spinel structure are themost important materials for negative temperature coefficient (NTC) thermistors. How toprepare the NTC thick film and thin film thermistors with high performance is the hot spot inNTC research area. The studies on the electronic conduction mechanism in polycrystallineNTC film thermistors are the difficult and key points in exploring the intrinsic mechanism.
The main research targets of this thesis are the manganite based NTC thermistors withspinel structure. The main objectives of our work are to prepare NTC film thermistors andmake clear the electronic conduction mechanism in polycrystalline NTC film thermistors.Based on a large number of experimental data on NTC bulk thermistors, a series of workswere conducted by employing screen printing method to prepare NTC thin film thermistors,spin-coating method to prepare NTC thin films, and temperature-dependent ac impedancespectra to analyze the conduction mechasnism. We systematically studied the effects oftechnological parameters of NTC bulk, thick film and thin film thermistors on their propertiesand intrinsic conduction mechanism by taking the small-polaron hopping conduction astheoretical basis.
The influences of chemical composition, sintering temperature and powder preparationmethod on the microstructure and electrical properties were studied on the Mn-Ni-O binary,Mn-Co-Ni-O ternary and Mn-Co-Ni-Cu-O quaternion systems. The results showed that theNi_(0.85)Co_(0.3)Mn_(1.85)O_4(MCN) bulk thermistors fabricated with powder by sol-gel method andsintered at1180oC for3h had much better performances than those with powder bytraditional solid-state reaction method.
Based on the experimental results of bulk thermistors, the MCN thick film thermistorswere prepared on Al_2O_3substrates by screen printing method. The effects of solid content(50%,67%and75%), sintering temperature (1150,1180and1200oC) and the shape ofelectrodes (terminal and interdigital) on the microstructure and electrical properties werediscussed in detail. The results demonstrated that the best performance could be obtained forMCN thick film thermistors with67%solid content and sintered at1180oC. The R-T relationof MCN thick film thermistors with terminal electrodes seemed to follow an exponential law(R=R0exp(B/T)), however, the R-T relation of MCN thick film thermistors with interdigitatedelectrodes seemed to follow linear relation (R=R0+AT). To further investigate the influence ofelectrode shape on the R-T relation, it was known that the exponential R-T relation forterminal electrodes was not affect by the breadth of terminal electrodes, and the linear R-T relation with interdigitated electrodes was not affect by the interval of fingers. Evidently, thelinear R-T relation should be attributed to the length of finger (a value). To decrease the avalue, it was seen clearly that the R-T relation of MCN thick film thermistors evolvedgradually from linear to exponential. The electric potential and field distribution in MCNthick films with different shape electrodes were analyzed simply by using the software Ansoftmaxwell12.
For MCN thin film thermistors prepared by spin-coating method on Al_2O_3substrates, theeffects of annealing temperature and thickness on the microstructure and electrical propertieswere studied. It was found that the MCN thin film thermistor annealed at750°C had lowerresistance (R_(25)=4.8MΩ), higher characteristic temperature (T_0=3720.6K), and small agingcoefficient (ΔR/R=3.7%) after aging at150°C for360h. The T_0and aging coefficient wasnot affected by the thickness of the thin film. The R_(25)was linearly decreasing with theincreasing of thickness. In order to reduce the R_(25), the Ni_(0.85)Co_(0.3)CuxMn_(1.85-x)O_4(MCCN，x=0，0.15，0.3and0.45) thin film thermistors were prepared on Al_2O_3substrates by sol-gel methodat700°C, and the effects of chemical composition on the microstructure and electricalproperties were studied. Ni0.85Co0.3Cu0.15Mn1.7O4seemed to be the optimum composition forthe MCCN thin films with R_(25) of0.56MΩ, T_0of4107.0K and Δ R/R of5.7%.
Through the analysis of temperature-dependent ac impedances of the NTC thick filmthermistors with different interdigitated electrode length (a value), the R-T behaviors of grainboundary (GB) and grain were obtained. The resistance of GB (R_(gb)) was higher than thate ofgrain (R_g); the hopping type of electrons in the grain is Variable-Range-Hopping (VRH); theR_gand T_0gare decreasing with the increasing of the a value. With the decreasing of the a value,the R_(gb)-T relation will evolve gradually from linear to exponential, which is the main reasonfor the changes of R-T relation of MCN thick film thermistors.
By the analysis of temperature-dependent ac impedances of MCN thin film thermistors,the grain size influence on the conductions of grain and GB was obtained. The conductionmechanisms of grain and GB both followed the small-polaron hopping model. In all samples,the R_(gb)was greater than the R_g, indicating the GB was of dominated resistance. The T_0gwaslarger than T_0gbimplying that the grain was of dominated characteristic temperature. Thehopping type of GBs was probably by Nearest-Neighbor-Hopping (NNH), and that of grainmight be a transition from VRH to NNH. We suggest that the samples are the systems withmixed NNH and VRH, and the electrical conductions of the samples are dominated by NNH.
These studies on the technological parameters and the electronic conduction mechanisms of NTC thick and thin film thermistors will be beneficial for the component design andindustrial applications.
本文选择Mn系尖晶石NTC体系为主要研究对象；以实现NTC热敏电阻的膜状化和解决多晶膜状NTC热敏电阻导电机理中的难点为主要研究目标；在大量块体NTC热敏电阻的实验数据为基础上，以丝网印刷法制备厚膜NTC热敏电阻、溶胶-凝胶法制备薄膜NTC热敏电阻和变温复阻抗谱分析多晶膜状NTC热敏电阻的导电机理为主要技术途径，开展了一系列的研究工作。对块体、厚膜和薄膜NTC热敏电阻的制备工艺参数进行了较系统的研究；以小极化子跳跃导电理论为基础，采用复阻抗谱的方法分析了影响厚膜和薄膜NTC热敏电阻性能的主要工艺参数对其导电机理的影响。
首先，研究了组分、烧结温度和粉体制备方法对Mn-Ni-O二元系、Mn-Co-Ni-O三元系和Mn-Co-Ni-Cu-O四元系块体热敏电阻的微结构和电性能的影响，结果表明：采用溶胶-凝胶法合成的粉体，烧结温度为1180oC，保温时间为3h，组分为Ni_(0.85)Co_(0.3)Mn_(1.85)O_4(MCN)的块体热敏电阻各项性能均较优异。
其次，基于块体NTC热敏电阻实验数据，采用丝网印刷法在Al_2O_3基底上制备了MCN厚膜热敏电阻，讨论了固含量(50%、67%和75%)、烧结温度(1150、1180和1200oC)和电极形状(端电极和叉指电极)对MCN厚膜热敏电阻微结构和电性能的影响。结果表明：固含量为67%，烧结温度为1180oC时，制备有端电极和叉指电极的MCN厚膜热敏电阻的性能均较优异。采用端电极的MCN厚膜R-T关系满足指数关系(R=R0exp(B/T))，而采用叉指电极的厚膜热敏电阻的R-T关系为线性关系(R=R0+AT)。分析了电极形状对MCN厚膜热敏电阻R-T关系的影响：端电极MCN厚膜热敏电阻，端电极的宽度并不会影响其R-T关系的指数关系；叉指电极MCN厚膜热敏电阻，叉指间距离的改变不会影响其R-T关系的线性关系；叉指长度(a值)的大小是影响其R-T关系的主要原因；当a值变小时，厚膜热敏电阻的R-T关系由开始的线性关系慢慢过渡到指数关系。采用Ansoft maxwell12软件对MCN厚膜的电势能和电场分布进行了简单的分析。
第三，采用溶胶-凝胶法在Al_2O_3基底上成功制备了MCN薄膜热敏电阻。研究了退火温度(650、700、750和800°C)和薄膜厚度(519.6、627.8和742.3nm)对MCN薄膜微结构和电性能的影响。对于MCN薄膜热敏电阻而言，750°C为最佳的退火温度。750°C下制备的MCN薄膜热敏电阻的室温电阻R_(25)=4.8MΩ，特征温度T_0=3720.6K，老化系数ΔR/R=3.7%。厚度对MCN薄膜热敏电阻的T_0值影响不大；样品R_(25)随着厚度的增加而减小，近似于线性减小；厚度对MCN薄膜热敏电阻的老化系数影响不大。为了达到减小电阻值的目的，采用溶胶-凝胶法在Al_2O_3基底上，700°C退火温度下，成功制备了Ni_(0.85)Co_(0.3)CuxMn_(1.85-x)O_4(MCCN，x=0，0.15，0.3和0.45)薄膜，研究了组分对MCCN薄膜热敏电阻的微观结构和电性能的影响。对于MCCN薄膜热敏电阻而言，当x=0.15，MCCN热敏电阻的R_(25)较小(0.56MΩ)，灵敏度较高(T_0=4107.0K)，老化系数较小(ΔR/R=5.7%)，为较合适的组分。
第四，通过对具有不同叉指长度(a值)的叉指电极MCN厚膜热敏电阻的变温复阻抗谱的分析，我们得到了具有不同a值的MCN厚膜热敏电阻中晶粒与晶界的R-T特性。样品中晶界电阻(R_(gb))均大于晶粒电阻(R_g)；晶粒内部电子的输运为变程跳跃(VRH)；a值越大，晶粒电阻和特征温度越小；当a值变小时，样品晶界的R_(gb)-T关系由开始的线性关系慢慢过渡到指数关系，这是引起厚膜热敏电阻R-T关系随a值大小发生变化的主要原因。
第五，通过对不同晶粒尺寸的MCN薄膜热敏电阻变温复阻抗谱的分析，我们得到了：在不同晶粒尺寸的MCN薄膜热敏电阻中，晶粒与晶界处电子的导电均为跳跃导电； R_(gb)均大于R_g，这说明材料的电阻由晶界主导；而晶粒特征温度(T_0~g)均大于晶界特征温度(T_0gb)，这说明材料中特征温度由晶粒主导。晶界的电子跳跃形式为最近邻跳跃(NNH)，而晶粒内部电子的跳跃形式为由VRH向NNH过渡的跳跃方式，薄膜热敏电阻中电子跳跃形式为NNH主导的，VRH和NNH相结合的跳跃形式。
NTC厚膜和薄膜热敏电阻制备工艺参数的研究以及内部导电机理的分析将为NTC厚膜和薄膜的工业应用提供有意义的指导。
Manganite based transition metal oxide ceramics with AB_2O_4spinel structure are themost important materials for negative temperature coefficient (NTC) thermistors. How toprepare the NTC thick film and thin film thermistors with high performance is the hot spot inNTC research area. The studies on the electronic conduction mechanism in polycrystallineNTC film thermistors are the difficult and key points in exploring the intrinsic mechanism.
The main research targets of this thesis are the manganite based NTC thermistors withspinel structure. The main objectives of our work are to prepare NTC film thermistors andmake clear the electronic conduction mechanism in polycrystalline NTC film thermistors.Based on a large number of experimental data on NTC bulk thermistors, a series of workswere conducted by employing screen printing method to prepare NTC thin film thermistors,spin-coating method to prepare NTC thin films, and temperature-dependent ac impedancespectra to analyze the conduction mechasnism. We systematically studied the effects oftechnological parameters of NTC bulk, thick film and thin film thermistors on their propertiesand intrinsic conduction mechanism by taking the small-polaron hopping conduction astheoretical basis.
The influences of chemical composition, sintering temperature and powder preparationmethod on the microstructure and electrical properties were studied on the Mn-Ni-O binary,Mn-Co-Ni-O ternary and Mn-Co-Ni-Cu-O quaternion systems. The results showed that theNi_(0.85)Co_(0.3)Mn_(1.85)O_4(MCN) bulk thermistors fabricated with powder by sol-gel method andsintered at1180oC for3h had much better performances than those with powder bytraditional solid-state reaction method.
Based on the experimental results of bulk thermistors, the MCN thick film thermistorswere prepared on Al_2O_3substrates by screen printing method. The effects of solid content(50%,67%and75%), sintering temperature (1150,1180and1200oC) and the shape ofelectrodes (terminal and interdigital) on the microstructure and electrical properties werediscussed in detail. The results demonstrated that the best performance could be obtained forMCN thick film thermistors with67%solid content and sintered at1180oC. The R-T relationof MCN thick film thermistors with terminal electrodes seemed to follow an exponential law(R=R0exp(B/T)), however, the R-T relation of MCN thick film thermistors with interdigitatedelectrodes seemed to follow linear relation (R=R0+AT). To further investigate the influence ofelectrode shape on the R-T relation, it was known that the exponential R-T relation forterminal electrodes was not affect by the breadth of terminal electrodes, and the linear R-T relation with interdigitated electrodes was not affect by the interval of fingers. Evidently, thelinear R-T relation should be attributed to the length of finger (a value). To decrease the avalue, it was seen clearly that the R-T relation of MCN thick film thermistors evolvedgradually from linear to exponential. The electric potential and field distribution in MCNthick films with different shape electrodes were analyzed simply by using the software Ansoftmaxwell12.
For MCN thin film thermistors prepared by spin-coating method on Al_2O_3substrates, theeffects of annealing temperature and thickness on the microstructure and electrical propertieswere studied. It was found that the MCN thin film thermistor annealed at750°C had lowerresistance (R_(25)=4.8MΩ), higher characteristic temperature (T_0=3720.6K), and small agingcoefficient (ΔR/R=3.7%) after aging at150°C for360h. The T_0and aging coefficient wasnot affected by the thickness of the thin film. The R_(25)was linearly decreasing with theincreasing of thickness. In order to reduce the R_(25), the Ni_(0.85)Co_(0.3)CuxMn_(1.85-x)O_4(MCCN，x=0，0.15，0.3and0.45) thin film thermistors were prepared on Al_2O_3substrates by sol-gel methodat700°C, and the effects of chemical composition on the microstructure and electricalproperties were studied. Ni0.85Co0.3Cu0.15Mn1.7O4seemed to be the optimum composition forthe MCCN thin films with R_(25) of0.56MΩ, T_0of4107.0K and Δ R/R of5.7%.
Through the analysis of temperature-dependent ac impedances of the NTC thick filmthermistors with different interdigitated electrode length (a value), the R-T behaviors of grainboundary (GB) and grain were obtained. The resistance of GB (R_(gb)) was higher than thate ofgrain (R_g); the hopping type of electrons in the grain is Variable-Range-Hopping (VRH); theR_gand T_0gare decreasing with the increasing of the a value. With the decreasing of the a value,the R_(gb)-T relation will evolve gradually from linear to exponential, which is the main reasonfor the changes of R-T relation of MCN thick film thermistors.
By the analysis of temperature-dependent ac impedances of MCN thin film thermistors,the grain size influence on the conductions of grain and GB was obtained. The conductionmechanisms of grain and GB both followed the small-polaron hopping model. In all samples,the R_(gb)was greater than the R_g, indicating the GB was of dominated resistance. The T_0gwaslarger than T_0gbimplying that the grain was of dominated characteristic temperature. Thehopping type of GBs was probably by Nearest-Neighbor-Hopping (NNH), and that of grainmight be a transition from VRH to NNH. We suggest that the samples are the systems withmixed NNH and VRH, and the electrical conductions of the samples are dominated by NNH.
These studies on the technological parameters and the electronic conduction mechanisms of NTC thick and thin film thermistors will be beneficial for the component design andindustrial applications.
引文
[1] Park K., Han I.H., Effect of Al2O3addition on the microstructure and electricalproperties of (Mn0.37Ni0.3Co0.33xAlx)O4(0≤x≤0.03) NTC thermistors [J]. MaterialsScience and Engineering B.2005,119:55–60
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