Ta及Ta-O薄膜的制备及其电学性能研究
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摘要
本文采用磁控溅射方法在玻璃基底上制备了纯Ta薄膜和低值Ta-0薄膜。研究了不同制备工艺参数以及热处理过程中上述两种成分薄膜的微观结构、表面形貌以及化学组成的演变及其对电性能的影响。同时研究了n与Ta0_x缓冲层的微观结构、表面特性及其对沉积其上的Ta薄膜微观结构的影响，分析了缓冲层对Ta薄膜的生长机理以及Ta/n和Ta/Ta0_x薄膜微观结构的演变对电学性能的影响。
溅射功率、沉积温度对Ta薄膜的沉积速率、结晶取向、0/Ta比值以及电性能起着重要作用；所沉积的Ta薄膜均呈现碳污染。随溅射功率的增加，Ta薄膜的沉积速率几乎呈线性增大，薄膜中晶粒取向增多，颗粒尺寸增大，杂质碳原子含量基本不变，0/Ta比值减小，导电性能增加，TcR住正值方向偏移。在300℃～500℃范围沉积的Ta薄膜均为p-Ta，择优取向为p-Ta(200)，基底温度增加到650℃，部分B-Ta转化为α-Ta，电阻率迅速下降。随着基底温度的升高，Ta薄膜的表面平均粗糙度和颗粒尺寸变小，致密度提高，0/Ta原子比值减小，电阻率减小。
不同热处理工艺对Ta薄膜的微观结构、表面特性与相的组成有重要影响，进而影响其电性能。在O-2Pa低真空环境中热处理，其室温电阻率随着热处理温度的上升，呈先上升、后略微下降趋势；而在O-2Pa02中热处理，其室温电阻率随热处理温度的上升而增大。相同的热处理温度，在02中热处理后的Ta薄膜室温电阻率都要比在低真空下热处理后的电阻率大。薄膜热处理后微观结构对电性能的影响机理可以采用简单化的双层并联电阻模型，借助双导电特性来定性解释。
Ta-0薄膜的微观结构、化学组成与溅射气氛中的0z含量有关。随着溅射气体中02含量的增加，薄膜的结晶相含量迅速减少。650℃高温热处理促进Ta-0薄膜发生结晶析出；Ta-0薄膜中氧的含量及微观结构的演变对电性能起主导作用。真空环境下的电阻-温度曲线随薄膜中氧含量的增加由近似线性关系逐渐演变为近似指数形式，空气环境下的电阻-温度特性曲线表现为冷却时的电阻变化曲线斜率要比加热时的斜率更负。
对比研究了不同厚度及氧含量的Ta-0薄膜经不同温度、气氛和时间老化后的电学稳定性能。不同厚度的Ta-0薄膜，其AR/R值随着老化时间及温度的增加而增大。Ta-0薄膜在空气环境中经相同温度及时间老化后，其相对电阻变化(AR/R)值随溅射气体中0：含量的增加而增大；Ta-0薄膜存在老化稳定性较差的问题。Ta-0薄膜在空气或氧气气氛下老化处理后微观结构对电性能的影响机理可以用颗粒边界氧扩散-氧化模型来定性解释。
沉积于玻璃和Si(111)基底的Ta/n薄膜，其各结晶相的体积分数部受Ti缓冲层厚度的影响。n缓冲层的引入能有效抑制Ta薄膜中B-Ta相的生长，而促进α-Ta相的形成。将Ti缓冲层暴露于空气环境后，沉积的Ta薄膜由α-Ta相和β-Ta相组成，其中β-Ta分别呈(200)与(004)晶面择优取向生长，α-Ta仍以(110)晶面择优取向生长。Ti缓冲层对Ta薄膜的生长的影响机理，可用n缓冲层与Ta薄膜之间的晶格匹配来解释。
Ta0X缓冲层的微观结构与表面形貌对Ta薄膜的微观结构、颗粒尺寸、表面形貌以及断面形貌有重要影响，进而影响其电性能。随着0_2/Ar流量比值的增加，Ta0_x缓冲层的结晶颗粒迅速减少，薄膜逐渐由晶态成分逐渐转变为非晶态成分占主导地位，使沉积其上的Ta薄膜的结晶取向性变差，粒度减小，Ta薄膜与Ta0_x缓冲层之间逐渐出现明显的分界面。Ta/Ta0_x薄膜内Ta颗粒的减小，使薄膜内晶界密度增加，从而增强晶界电子散射效应，使Ta/Ta0_x薄膜的室温电阻率增加。
In this paper, Ta and Ta-O films were deposited on glass substrates by direct current magnetron sputtering. The microstructure, surface morphology and chemical composition evolution of two types of the films were investigated as a function of sputtering parameters and heat treatment procedure, and the effects of microstructure, surface morphology and chemical composition on the electrical properties of the films was also be studied. The microstructure and surface characteristics of Ti and TaO×buffer layer films were researched, and the effects of microstrure and surface characteristics on the tantalum films deposited on them were also investigated. The grown model of the tantalum films deposited on Ti and TaO×buffer layer films was analyzed. Furthermore, it was also studied that the effects of microstructure evolution on electrical properties of the Ta/Ti and Ta/TaO×films in this paper.
Sputtering power and substrate temperature play a significant role on the deposition rate, crystal orientation, O/Ta ratio and electrical properties of Ta films. All Ta films in our study show the presence of carbon contamination. As increasing sputtering power, the carbon atomic content in films keeps no change, but the deposition rate of Ta films increases linearly nearly, tantalum films show more growth orientation and the grain size in films becomes large and the O/Ta ratio of the films decreases, which increases the conductivity and causes the TCR to shift positive value. The tantalum film was composed of ratio of the tantalum films decreased and the density of the tantalum films increased, which all make the resistivity decreased.
Different heat treating procedure plays an important role on the microstructure, surface properties and crystal phase of tantalum films, which influence their electrical properties. The electrical resistivity at room temperature of tantalum films annealed at low vacuum of 0.2Pa is continuous increased at the beginning and then decreased gradually as increasing the annealing temperature. However, the electrical resistivity at room temperature of tantalum films annealed at O_2 ambience of 0.2Pa is increased rapidly as increasing the annealing temperature. At the same annealing temperature, the electrical resistivity values at room temperature of tantalum films annealing at0.2Pa O_2 ambience are larger than that annealing at low vacuum of 0.2Pa. The effect ofthe microstructure on the electrical properties of tantalum films after annealed atdifferent procedure can be explained by a simple double layer parallel connectionresistance model and dual conduction model.
The microsture and chemical compositiom of Ta-O films depends on the relativerates at which oxygen is leaked into the sputtering system. As increasing the flow ratesof oxygen, the incrystal phase content of Ta-O films decreased rapidly. The -vs-Tcurve in vacuum ambience transformed from closely linear to exponential behaviourwith increasing the oxygen content of the films. However, in atmosphere ambience, theslope of the -vs-T curve for heating process was more negative than that for coolingprocess. The value of relative resistance change ( DR R ) was increased with the higheroxygen flow rate.
It was investigated that the electrical stability of Ta-O films with differentthickness and oxygen content after aging at different temperature, ambience and time.The value of relative resistance change ( DRR ) of Ta-O films with different thicknesswas increased as increasing aging time and temperature. At the same temperature andtime, the value of relative resistance change ( DRR ) of Ta-O films aged in atmospherewas increased with the increase of oxygen flow rate during deposition. The Ta-O filmsshowed poor aging stability. The effect of the microstructure on the electricalproperties of Ta-O films after aged in atmosphere or oxygen ambience can be made aqualitative explaination by an oxygen diffusion-oxidation of grain boundary model.
The volume fraction of the nanocrystalline phase of Ta/Ti films deposited on glassor Si (111) substrate was influenced from the thickness of Ti buffer layer. The Ti bufferlayer can effectively inhibit the formation of the Ta phase and promote the -Taphase growth in Ta films. When the Ti buffer layer was exposed to atmosphereambience, the Ta films were all composed of Ta phase which still grown at the -Ta(110) preferred orientation and Ta phase which grown at the Ta (200) and Ta(004) preferred orientation, respectively. The effect of Ti buffer layer on the growth ofTa films can be explained by the crystal lattice match between the Ti buffer and Tafilms.
The microstructure and surface morphology of TaO×duffer layer play animportant role on the microstructure, grain size, surface and cross-sectional propertiesof Ta films, which influence thier electrical properties. As increasing the O_2/Ar flowrate, the amount of crystal grains in the TaO×duffer layer decreased rapidly, the dominant component in films changed from crystalline phase to amorphous phase, which reduced the crystal orientation and decreased the Ta crystalline granular size of film deposited on it, and showed an abvious interface between Ta film and TaO×duffer layer. The decrease of the Ta crystalline granular size in Ta/TaO×films would increase the crystalline boundary density in the films and enchance electron scattering effect among the crystalline boundary, which increased the room temperature resistivity of Ta/TaO×films.
溅射功率、沉积温度对Ta薄膜的沉积速率、结晶取向、0/Ta比值以及电性能起着重要作用；所沉积的Ta薄膜均呈现碳污染。随溅射功率的增加，Ta薄膜的沉积速率几乎呈线性增大，薄膜中晶粒取向增多，颗粒尺寸增大，杂质碳原子含量基本不变，0/Ta比值减小，导电性能增加，TcR住正值方向偏移。在300℃～500℃范围沉积的Ta薄膜均为p-Ta，择优取向为p-Ta(200)，基底温度增加到650℃，部分B-Ta转化为α-Ta，电阻率迅速下降。随着基底温度的升高，Ta薄膜的表面平均粗糙度和颗粒尺寸变小，致密度提高，0/Ta原子比值减小，电阻率减小。
不同热处理工艺对Ta薄膜的微观结构、表面特性与相的组成有重要影响，进而影响其电性能。在O-2Pa低真空环境中热处理，其室温电阻率随着热处理温度的上升，呈先上升、后略微下降趋势；而在O-2Pa02中热处理，其室温电阻率随热处理温度的上升而增大。相同的热处理温度，在02中热处理后的Ta薄膜室温电阻率都要比在低真空下热处理后的电阻率大。薄膜热处理后微观结构对电性能的影响机理可以采用简单化的双层并联电阻模型，借助双导电特性来定性解释。
Ta-0薄膜的微观结构、化学组成与溅射气氛中的0z含量有关。随着溅射气体中02含量的增加，薄膜的结晶相含量迅速减少。650℃高温热处理促进Ta-0薄膜发生结晶析出；Ta-0薄膜中氧的含量及微观结构的演变对电性能起主导作用。真空环境下的电阻-温度曲线随薄膜中氧含量的增加由近似线性关系逐渐演变为近似指数形式，空气环境下的电阻-温度特性曲线表现为冷却时的电阻变化曲线斜率要比加热时的斜率更负。
对比研究了不同厚度及氧含量的Ta-0薄膜经不同温度、气氛和时间老化后的电学稳定性能。不同厚度的Ta-0薄膜，其AR/R值随着老化时间及温度的增加而增大。Ta-0薄膜在空气环境中经相同温度及时间老化后，其相对电阻变化(AR/R)值随溅射气体中0：含量的增加而增大；Ta-0薄膜存在老化稳定性较差的问题。Ta-0薄膜在空气或氧气气氛下老化处理后微观结构对电性能的影响机理可以用颗粒边界氧扩散-氧化模型来定性解释。
沉积于玻璃和Si(111)基底的Ta/n薄膜，其各结晶相的体积分数部受Ti缓冲层厚度的影响。n缓冲层的引入能有效抑制Ta薄膜中B-Ta相的生长，而促进α-Ta相的形成。将Ti缓冲层暴露于空气环境后，沉积的Ta薄膜由α-Ta相和β-Ta相组成，其中β-Ta分别呈(200)与(004)晶面择优取向生长，α-Ta仍以(110)晶面择优取向生长。Ti缓冲层对Ta薄膜的生长的影响机理，可用n缓冲层与Ta薄膜之间的晶格匹配来解释。
Ta0X缓冲层的微观结构与表面形貌对Ta薄膜的微观结构、颗粒尺寸、表面形貌以及断面形貌有重要影响，进而影响其电性能。随着0_2/Ar流量比值的增加，Ta0_x缓冲层的结晶颗粒迅速减少，薄膜逐渐由晶态成分逐渐转变为非晶态成分占主导地位，使沉积其上的Ta薄膜的结晶取向性变差，粒度减小，Ta薄膜与Ta0_x缓冲层之间逐渐出现明显的分界面。Ta/Ta0_x薄膜内Ta颗粒的减小，使薄膜内晶界密度增加，从而增强晶界电子散射效应，使Ta/Ta0_x薄膜的室温电阻率增加。
In this paper, Ta and Ta-O films were deposited on glass substrates by direct current magnetron sputtering. The microstructure, surface morphology and chemical composition evolution of two types of the films were investigated as a function of sputtering parameters and heat treatment procedure, and the effects of microstructure, surface morphology and chemical composition on the electrical properties of the films was also be studied. The microstructure and surface characteristics of Ti and TaO×buffer layer films were researched, and the effects of microstrure and surface characteristics on the tantalum films deposited on them were also investigated. The grown model of the tantalum films deposited on Ti and TaO×buffer layer films was analyzed. Furthermore, it was also studied that the effects of microstructure evolution on electrical properties of the Ta/Ti and Ta/TaO×films in this paper.
Sputtering power and substrate temperature play a significant role on the deposition rate, crystal orientation, O/Ta ratio and electrical properties of Ta films. All Ta films in our study show the presence of carbon contamination. As increasing sputtering power, the carbon atomic content in films keeps no change, but the deposition rate of Ta films increases linearly nearly, tantalum films show more growth orientation and the grain size in films becomes large and the O/Ta ratio of the films decreases, which increases the conductivity and causes the TCR to shift positive value. The tantalum film was composed of ratio of the tantalum films decreased and the density of the tantalum films increased, which all make the resistivity decreased.
Different heat treating procedure plays an important role on the microstructure, surface properties and crystal phase of tantalum films, which influence their electrical properties. The electrical resistivity at room temperature of tantalum films annealed at low vacuum of 0.2Pa is continuous increased at the beginning and then decreased gradually as increasing the annealing temperature. However, the electrical resistivity at room temperature of tantalum films annealed at O_2 ambience of 0.2Pa is increased rapidly as increasing the annealing temperature. At the same annealing temperature, the electrical resistivity values at room temperature of tantalum films annealing at0.2Pa O_2 ambience are larger than that annealing at low vacuum of 0.2Pa. The effect ofthe microstructure on the electrical properties of tantalum films after annealed atdifferent procedure can be explained by a simple double layer parallel connectionresistance model and dual conduction model.
The microsture and chemical compositiom of Ta-O films depends on the relativerates at which oxygen is leaked into the sputtering system. As increasing the flow ratesof oxygen, the incrystal phase content of Ta-O films decreased rapidly. The -vs-Tcurve in vacuum ambience transformed from closely linear to exponential behaviourwith increasing the oxygen content of the films. However, in atmosphere ambience, theslope of the -vs-T curve for heating process was more negative than that for coolingprocess. The value of relative resistance change ( DR R ) was increased with the higheroxygen flow rate.
It was investigated that the electrical stability of Ta-O films with differentthickness and oxygen content after aging at different temperature, ambience and time.The value of relative resistance change ( DRR ) of Ta-O films with different thicknesswas increased as increasing aging time and temperature. At the same temperature andtime, the value of relative resistance change ( DRR ) of Ta-O films aged in atmospherewas increased with the increase of oxygen flow rate during deposition. The Ta-O filmsshowed poor aging stability. The effect of the microstructure on the electricalproperties of Ta-O films after aged in atmosphere or oxygen ambience can be made aqualitative explaination by an oxygen diffusion-oxidation of grain boundary model.
The volume fraction of the nanocrystalline phase of Ta/Ti films deposited on glassor Si (111) substrate was influenced from the thickness of Ti buffer layer. The Ti bufferlayer can effectively inhibit the formation of the Ta phase and promote the -Taphase growth in Ta films. When the Ti buffer layer was exposed to atmosphereambience, the Ta films were all composed of Ta phase which still grown at the -Ta(110) preferred orientation and Ta phase which grown at the Ta (200) and Ta(004) preferred orientation, respectively. The effect of Ti buffer layer on the growth ofTa films can be explained by the crystal lattice match between the Ti buffer and Tafilms.
The microstructure and surface morphology of TaO×duffer layer play animportant role on the microstructure, grain size, surface and cross-sectional propertiesof Ta films, which influence thier electrical properties. As increasing the O_2/Ar flowrate, the amount of crystal grains in the TaO×duffer layer decreased rapidly, the dominant component in films changed from crystalline phase to amorphous phase, which reduced the crystal orientation and decreased the Ta crystalline granular size of film deposited on it, and showed an abvious interface between Ta film and TaO×duffer layer. The decrease of the Ta crystalline granular size in Ta/TaO×films would increase the crystalline boundary density in the films and enchance electron scattering effect among the crystalline boundary, which increased the room temperature resistivity of Ta/TaO×films.
引文
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