单晶硅基LaB_6薄膜的磁控溅射制备工艺及生长机制
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摘要
LaB6具有良好的导电性、热稳定性和化学稳定性,具有可恒定地维持一个活性的阴极表面,是作为阴极发射体的理想材料。大尺寸LaB6棒状阴极制备工艺比较困难,大面积的LaB6多晶薄膜则更为经济实用。国内外对LaB6薄膜的研究主要以金属玻璃、聚合物等为基体,以探求LaB6薄膜的发射性能及光学性能,对LaB6薄膜作为场发射平板显示器用电子发射极的研究较少。单晶Si是作为基体研究薄膜最理想的材料,在Si基体表面制备出取向一致的LaB6薄膜是制作平面和尖锥场发射器件的基础。而在不同单晶晶向Si基体上制备LaB6薄膜的空白凸现出基础研究的必要性。
本论文利用磁控溅射法在(111)单晶晶向Si基片上制备出LaB6薄膜,并系统研究了溅射功率、氩气气压、基片偏压、基片温度和溅射时间对LaB6薄膜沉积速率、晶体结构和形貌的影响；在此基础上优化工艺参数,制备出结晶度高的LaB6薄膜；分析了退火温度对LaB6薄膜分子结构和结晶度的影响；对不同单晶晶向Si(111)和Si(100)基底上制备的LaB6薄膜元素组成、晶体结构和组织形貌进行了分析；并系统研究了不同工艺参数下制备LaB6薄膜与基体的结合强度、纳米硬度及弹性模量、导电性能；最后初步探讨了LaB6薄膜的高温抗氧化性。
研究结果表明,溅射功率为44 W,氩气气压为1.0 Pa,基片偏压为-100 V,基片温度为400℃时制备的LaB6薄膜表面平整,结构致密,结晶度最高且LaB6(100)晶面发生明显的优生生长。溅射时间超过20 min时,薄膜出现LaB6晶体结构,衍射峰的峰形宽化且弥散,结晶度低；随着溅射时间的增加,XRD衍射峰强度显著增强,结晶度提高；LaB6薄膜呈柱状生长,生长方向垂直于基底的方向,LaB6薄膜与基底之间没有化学反应以及化合物的形成。
研究了不同退火温度对制备LaB6薄膜的结晶度影响。400℃保温1 h退火处理后薄膜开始由非晶向晶体转变,但只是部分转变为LaB6晶体。500℃退火处理后的薄膜结晶度高,颗粒较小,表面平整,薄膜LaB6(110)面有择优生长趋势。退火温度继续升高到600℃时,LaB6薄膜的衍射峰宽化而弥散,结晶度降低,颗粒异常长大、团聚。
分析了不同单晶晶向Si(111)和Si(100)基底对LaB6薄膜晶体结构、元素组成和组织形貌的影响。结果表明,不同单晶晶向Si(111)和Si(100)基底上制备的薄膜LaB6(100)晶面均发生明显的优生生长,Si(111)基底上制备的LaB6簿膜结晶度更高；不同晶向单晶Si(111)和Si(100)基底上制备的LaB6薄膜的La和B的原子比分别为为1：4.12和1：2.75,大于理论比值1：6；单晶Si(111)基底上制备的LaB6薄膜在214 cm-1、685 cm-1、1100 cm-1和1242cm-1处共有四个拉曼散射峰,分别与T1u、T2g、Eg和Alg声子相对应；LaB6薄膜的拉曼峰形相对于微米粉末发生宽化,与LaB6晶格的畸变或内部应力有关。
高分辨电镜结果显示,LaB6薄膜主要为多晶结构,但存在非晶成分。薄膜存在LaB6(100)和LaB6(110)晶面,晶格产生了不同程度的晶格畸变,其晶面间距与其微米材料的晶面间距存在差值。在Si(111)和Si(100)基底上制备的薄膜均以LaB6[100]晶向为优先生长方向。
LaB6薄膜与基体间有良好的结合力,可达到最大值17.12 N(溅射功率：44 W,氩气气压：1.0 Pa,基片偏压为：100 V,基片温度：400℃,溅射时间：90 min)。LaB6薄膜的荷载-位移曲线均平滑、无突变,表明弹塑性良好,硬度与结晶度变化趋势一致,弹性模量随着晶粒尺寸的增大而减小。不同的工艺参数下制备的LaB6薄膜电阻率都很低,可达到最小值2.38Ω/□,其导电性能比块体材料稍弱。LaB6薄膜的高温抗氧化性远不及微米粉末,失重曲线在793.1℃出现明显的增重,即被氧化。
LaB6 has an excellent conductivity, thermal stability and chemical stability. It also has cathode surface which can maintain a constant activity, whcich is an ideal material as cathode emitter. It is hard to prepare large-scale LaB6 rode cathode. At the same time, it is economical and practical to prepare large area polycrystalline films. The recent research focus on the emissional and optical properties of LaB6 films deposited on metal, glass or polymer substrates. However, few studies were related with LaB6 films as field emission electron emitter of flat panel displays. Single crystal silicon is an ideal material as substrate for film's investigation. Preparation of LaB6 films with a particular growing direction on silicon substrate is the foundation of producing plane and tip field emission devices. At the same time, the absence of depositing LaB6 films on silicon substrate with different crystal directions highlighted the research significance for basic research.
In this paper, LaB6 films have been prepared on single crystal Si (111) substrate by magnetron sputtering method. The influence of sputtering power, argon pressure, substrate bias voltage, substrate temperature and sputtering time on the depositing rate, crystal structure and morphology of the LaB6 films has been investigated. Hence, we got the optimized processing parameter for preparing LaB6 films with good crystalline. The influence of annealing temperature on the deposition rate, molecular structure and crystalline of LaB6 has been studied. The influence of Si (111) and Si (100) substrate on the crystal structure, molecular structure, chemical composition and morphology of LaB6 films has been discussed. The dependence of bonding strength, nano-hardness, elastic modulus and electrical conductivity of the LaB6 films on the processing parameter was investigated systematically. Finally, we researched the high temperature thermal stability of LaB6 films.
The results showed that the LaB6 films had smooth surface, compact structure, high crystallization and distinct LaB6 (111) preferred orientation when deposited at the optimized parameters (sputtering power was 44 W, argon gas pressure was 1.0 Pa, substrate bias voltage was-100 V, substrate temperature was 400℃). The LaB6 films began to form crystallization structures when the sputtering time was more than 20 min. But the diffraction peaks were broaden and asymmetric, indicating that the crystalline was poor. As the sputtering time increasing, XRD peaks intensity increased significantly, and the crystallization improved. The LaB6 films presented a regular columnar growth pattern, with the direction perpendicular to the substrates. No chemical reactions or chemicals appeared between LaB6 films and the substrates.
The influence of annealing temperature on the crystallization of amorphous LaB6 films was investigated. Part of LaB6 films changed from amorphous to crystal after annealing process at 400℃lasting for 1 h. The films showed smaller particles, smoother surface and higher crystalline with LaB6(100) preferred orientation after annealing process at 500℃. When the annealing temperature increased to 600℃, the diffraction peaks of the LaB6 films broadened and dispersed, revealing poor crystalline. At the same time, the grains grew up abnormally and aggregated.
The crystal structure, morphology and molecular structure of LaB6 films deposited on Si (111) and Si (100) substrates were detected. The dominant orientation of films was LaB6 (100) on both substrates. At the same time, the crystalline of films was better and their LaB6 (100) showed more obviously preferred growth when the films were deposited on Si (111) substrate. The atomic ratio of La and B for the films which were deposited on Si (111) and Si (100) substrate was 1:4.12 and 1:2.75 respectively, which both higher than the theoretical ratio of 1:6. The LaB & films deposited on Si (111) substrate had four Raman scattering peaks at 214 cm-1,685 cm-1, 1100 cm-1 and 1242 cm-1, which was consistent with T1u, T2g, Eg and A1g phonon, respectively. The Raman scattering peaks for the LaB6 films which were deposited on Si (100) substrate were lower than those deposited on Si (111) substrate. In addition, the Raman peaks for LaB6 films were broaden than that for the micron powders, which may be related to lattice distortion or internal stress in LaB6 films.
High-resolution electron microscopy showed that the LaB6 films had polycrystalline structure with some amorphous component. LaB6 (100) and LaB6 (110) planes existed in the films, but their plane spacing had some differences comparing with that of the conventional materials. This is due to the lattice distortion in the LaB6 films. Both of the LaB6 films had [100] directions as the priority direction on Si (111) and Si (100) substrates.
All the LaB6 films had excellent bonding strength with the substrates. The film-substrate bonding strength could reach 17.12 N (sputtering power was 44 W, argon gas pressure was 1.0 Pa, substrate bias voltage was -100 V, substrate temperature was 400℃and sputtering time was 90 min). The load-displacement curves of the films were smooth without break, indicating that the LaB6 films had excellent elastic plastic properties. The changes in hardness of LaB6 films were consistent with their crystalline. And the elastic modulus of the films decreased as the grain size increased.
The LaB6 films had low resistivity under different sputtering process, and reached a minimum value of 2.38Ω/□. The electrical conductivity of the films was slightly lower than that of the bulk materials, which was between conductors and insulators. The weight-loss curve for the LaB6 films appeared apparently gain at 793.1℃, which indicated that the LaB6 films were oxidized. The high temperature oxidation resistance of the LaB6 films was inferior to the micron powders.
本论文利用磁控溅射法在(111)单晶晶向Si基片上制备出LaB6薄膜,并系统研究了溅射功率、氩气气压、基片偏压、基片温度和溅射时间对LaB6薄膜沉积速率、晶体结构和形貌的影响；在此基础上优化工艺参数,制备出结晶度高的LaB6薄膜；分析了退火温度对LaB6薄膜分子结构和结晶度的影响；对不同单晶晶向Si(111)和Si(100)基底上制备的LaB6薄膜元素组成、晶体结构和组织形貌进行了分析；并系统研究了不同工艺参数下制备LaB6薄膜与基体的结合强度、纳米硬度及弹性模量、导电性能；最后初步探讨了LaB6薄膜的高温抗氧化性。
研究结果表明,溅射功率为44 W,氩气气压为1.0 Pa,基片偏压为-100 V,基片温度为400℃时制备的LaB6薄膜表面平整,结构致密,结晶度最高且LaB6(100)晶面发生明显的优生生长。溅射时间超过20 min时,薄膜出现LaB6晶体结构,衍射峰的峰形宽化且弥散,结晶度低；随着溅射时间的增加,XRD衍射峰强度显著增强,结晶度提高；LaB6薄膜呈柱状生长,生长方向垂直于基底的方向,LaB6薄膜与基底之间没有化学反应以及化合物的形成。
研究了不同退火温度对制备LaB6薄膜的结晶度影响。400℃保温1 h退火处理后薄膜开始由非晶向晶体转变,但只是部分转变为LaB6晶体。500℃退火处理后的薄膜结晶度高,颗粒较小,表面平整,薄膜LaB6(110)面有择优生长趋势。退火温度继续升高到600℃时,LaB6薄膜的衍射峰宽化而弥散,结晶度降低,颗粒异常长大、团聚。
分析了不同单晶晶向Si(111)和Si(100)基底对LaB6薄膜晶体结构、元素组成和组织形貌的影响。结果表明,不同单晶晶向Si(111)和Si(100)基底上制备的薄膜LaB6(100)晶面均发生明显的优生生长,Si(111)基底上制备的LaB6簿膜结晶度更高；不同晶向单晶Si(111)和Si(100)基底上制备的LaB6薄膜的La和B的原子比分别为为1：4.12和1：2.75,大于理论比值1：6；单晶Si(111)基底上制备的LaB6薄膜在214 cm-1、685 cm-1、1100 cm-1和1242cm-1处共有四个拉曼散射峰,分别与T1u、T2g、Eg和Alg声子相对应；LaB6薄膜的拉曼峰形相对于微米粉末发生宽化,与LaB6晶格的畸变或内部应力有关。
高分辨电镜结果显示,LaB6薄膜主要为多晶结构,但存在非晶成分。薄膜存在LaB6(100)和LaB6(110)晶面,晶格产生了不同程度的晶格畸变,其晶面间距与其微米材料的晶面间距存在差值。在Si(111)和Si(100)基底上制备的薄膜均以LaB6[100]晶向为优先生长方向。
LaB6薄膜与基体间有良好的结合力,可达到最大值17.12 N(溅射功率：44 W,氩气气压：1.0 Pa,基片偏压为：100 V,基片温度：400℃,溅射时间：90 min)。LaB6薄膜的荷载-位移曲线均平滑、无突变,表明弹塑性良好,硬度与结晶度变化趋势一致,弹性模量随着晶粒尺寸的增大而减小。不同的工艺参数下制备的LaB6薄膜电阻率都很低,可达到最小值2.38Ω/□,其导电性能比块体材料稍弱。LaB6薄膜的高温抗氧化性远不及微米粉末,失重曲线在793.1℃出现明显的增重,即被氧化。
LaB6 has an excellent conductivity, thermal stability and chemical stability. It also has cathode surface which can maintain a constant activity, whcich is an ideal material as cathode emitter. It is hard to prepare large-scale LaB6 rode cathode. At the same time, it is economical and practical to prepare large area polycrystalline films. The recent research focus on the emissional and optical properties of LaB6 films deposited on metal, glass or polymer substrates. However, few studies were related with LaB6 films as field emission electron emitter of flat panel displays. Single crystal silicon is an ideal material as substrate for film's investigation. Preparation of LaB6 films with a particular growing direction on silicon substrate is the foundation of producing plane and tip field emission devices. At the same time, the absence of depositing LaB6 films on silicon substrate with different crystal directions highlighted the research significance for basic research.
In this paper, LaB6 films have been prepared on single crystal Si (111) substrate by magnetron sputtering method. The influence of sputtering power, argon pressure, substrate bias voltage, substrate temperature and sputtering time on the depositing rate, crystal structure and morphology of the LaB6 films has been investigated. Hence, we got the optimized processing parameter for preparing LaB6 films with good crystalline. The influence of annealing temperature on the deposition rate, molecular structure and crystalline of LaB6 has been studied. The influence of Si (111) and Si (100) substrate on the crystal structure, molecular structure, chemical composition and morphology of LaB6 films has been discussed. The dependence of bonding strength, nano-hardness, elastic modulus and electrical conductivity of the LaB6 films on the processing parameter was investigated systematically. Finally, we researched the high temperature thermal stability of LaB6 films.
The results showed that the LaB6 films had smooth surface, compact structure, high crystallization and distinct LaB6 (111) preferred orientation when deposited at the optimized parameters (sputtering power was 44 W, argon gas pressure was 1.0 Pa, substrate bias voltage was-100 V, substrate temperature was 400℃). The LaB6 films began to form crystallization structures when the sputtering time was more than 20 min. But the diffraction peaks were broaden and asymmetric, indicating that the crystalline was poor. As the sputtering time increasing, XRD peaks intensity increased significantly, and the crystallization improved. The LaB6 films presented a regular columnar growth pattern, with the direction perpendicular to the substrates. No chemical reactions or chemicals appeared between LaB6 films and the substrates.
The influence of annealing temperature on the crystallization of amorphous LaB6 films was investigated. Part of LaB6 films changed from amorphous to crystal after annealing process at 400℃lasting for 1 h. The films showed smaller particles, smoother surface and higher crystalline with LaB6(100) preferred orientation after annealing process at 500℃. When the annealing temperature increased to 600℃, the diffraction peaks of the LaB6 films broadened and dispersed, revealing poor crystalline. At the same time, the grains grew up abnormally and aggregated.
The crystal structure, morphology and molecular structure of LaB6 films deposited on Si (111) and Si (100) substrates were detected. The dominant orientation of films was LaB6 (100) on both substrates. At the same time, the crystalline of films was better and their LaB6 (100) showed more obviously preferred growth when the films were deposited on Si (111) substrate. The atomic ratio of La and B for the films which were deposited on Si (111) and Si (100) substrate was 1:4.12 and 1:2.75 respectively, which both higher than the theoretical ratio of 1:6. The LaB & films deposited on Si (111) substrate had four Raman scattering peaks at 214 cm-1,685 cm-1, 1100 cm-1 and 1242 cm-1, which was consistent with T1u, T2g, Eg and A1g phonon, respectively. The Raman scattering peaks for the LaB6 films which were deposited on Si (100) substrate were lower than those deposited on Si (111) substrate. In addition, the Raman peaks for LaB6 films were broaden than that for the micron powders, which may be related to lattice distortion or internal stress in LaB6 films.
High-resolution electron microscopy showed that the LaB6 films had polycrystalline structure with some amorphous component. LaB6 (100) and LaB6 (110) planes existed in the films, but their plane spacing had some differences comparing with that of the conventional materials. This is due to the lattice distortion in the LaB6 films. Both of the LaB6 films had [100] directions as the priority direction on Si (111) and Si (100) substrates.
All the LaB6 films had excellent bonding strength with the substrates. The film-substrate bonding strength could reach 17.12 N (sputtering power was 44 W, argon gas pressure was 1.0 Pa, substrate bias voltage was -100 V, substrate temperature was 400℃and sputtering time was 90 min). The load-displacement curves of the films were smooth without break, indicating that the LaB6 films had excellent elastic plastic properties. The changes in hardness of LaB6 films were consistent with their crystalline. And the elastic modulus of the films decreased as the grain size increased.
The LaB6 films had low resistivity under different sputtering process, and reached a minimum value of 2.38Ω/□. The electrical conductivity of the films was slightly lower than that of the bulk materials, which was between conductors and insulators. The weight-loss curve for the LaB6 films appeared apparently gain at 793.1℃, which indicated that the LaB6 films were oxidized. The high temperature oxidation resistance of the LaB6 films was inferior to the micron powders.
引文
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