PECVD法低温制备二氧化硅薄膜(英文)

针对金属层间介质以及MEMS等对氧化硅薄膜的需求,介绍了采用等离子增强型化学气相沉积(PECVD)技术,以SiH4和N2O为反应气体,低温制备SiO2薄膜的方法.利用椭偏仪和应力测试系统对制得的SiO2薄膜的厚度、折射率、均匀性以及应力等性能指标进行了测试,探讨了射频功率、反应腔室压力、气体流量比等关键工艺参数对SiO2薄膜性能的影响.结果表明:SiO2薄膜的折射率主要由N2O/SiH4的流量比决定,而薄膜均匀性主要受电极间距以及反应腔室压力的影响.通过优化工艺参数,在低温260℃下制备了折射率为1.45～1.52、均匀性为±0.64%、应力在-350～-16MPa可控的SiO2薄膜.采用该方法制备的SiO2薄膜均匀性好、结构致密、沉积速率快、沉积温度低且应力可控,可广泛应用于集成电路以及MEMS器件中.     

分布式电子回旋共振等离子体制备高质量二氧化硅薄膜

介绍了一种采用DECR等离子体在低温下制备高质量SiO2薄膜的PECVD工艺。讨论了DECRPECVD工艺中气相O／Si原子比以及沉积速率对SiO2薄膜性能的影响。采用包括高能离子分析、椭偏仪、化学刻蚀以及红外吸收谱等物理和化学方法，对所镀SiO2薄膜的各种理化特性进行了分析和研究。在此基础上，还采用准静态I-U和高、低频C-U技术对优化工艺后的SiO2薄膜进行了电学性能测试，并在最后给出了采用DECRSiO2的薄膜晶体管的特性曲线。     

PECVD法玻璃容器内壁沉积SiO_2薄膜的SEM表征

采用自主研制的等离子体增强化学气相沉积(PECVD)专用设备,在玻璃容器内壁沉积SiO2薄膜,用作阻隔涂层。通过设计沉积工艺,在不同的气体流量比例、工作气压和生长时间等生长条件下制备出SiO2薄膜;通过扫描电子显微镜(SEM)测试表征薄膜的形貌和结构,评价薄膜的性能。根据表征结果分析了各种工艺参数对薄膜性能的影响,获得了较为优化的工艺参数,在玻璃容器内壁制备出较高质量的SiO2薄膜。     

用SiCl4／O2—PECVD技术低温沉积Si基厚SiO2薄膜

选取不含H2的SiCl4/O2混合气体作为反应源气体,并利用普通的PECVD技术来实现低温沉积Si基微米厚度的SiO2薄膜,测试并分析薄膜的红外吸收谱以及工艺参数对沉积过程的影响。     

白宝石上生长SiO2薄膜的工艺

用射频磁控反应溅射法,以高纯Si为靶材,高纯O2为反应气体,在白宝石上制备SiO2薄膜。对影响薄膜生长的工艺参数进行了分析,测试了薄膜的成分,并研究了薄膜的红外光学性能。结果表明,制备的薄膜中Si和O形成SiO2化学键,计算出的O与Si的原子比接近2:1,采用射频磁控反应溅射法在白宝石上能够沉积出SiO2薄膜。制备出的SiO2薄膜对白宝石衬底有较好的增透作用。     

硅靶中频反应磁控溅射二氧化硅薄膜的特性研究

报道了中频双靶反应磁控溅射制备二氧化硅（SiO2)薄膜的装置、工艺及薄膜特性。对制备的SiO2薄膜的化学配比和元素化学态进行了SAM和XPS分析，测试了膜层对钠离子（Na^ )阻挡性能、光学折射率和可见光的透过率。研究表明作者开发的中频双靶反应磁控溅射沉积SiO2薄膜的设备和工艺可以高速率、大面积制备高质量的SiO2膜。     

氧分压影响中频磁控溅射沉积SiO_2薄膜光学性能研究

采用中频反应磁控溅射沉积非晶二氧化硅(a_SiO2)薄膜,用X射线衍射、原子力显微镜、傅里叶红外光谱等方法研究氧分压影响退火前、后的两种SiO2薄膜样品的微观结构、折射率和消光系数等特性的变化规律。结果显示:室温下,沉积速率随氧分压的增大而减小,有利于提高薄膜的光滑性和致密度;在不同氧分压下沉积的SiO2薄膜均为非晶态结构;氧分压为25%时,薄膜表面具有均匀、光滑、致密的性能特征;折射率和消光系数都依赖于氧分压,氧分压大于15%时,薄膜在600 nm处的折射率n约为1.45～1.47,消光系数低于10-4。这表明适当提高氧分压有利于获得光学性能较好的SiO2薄膜。傅里叶红外吸收光谱测试表明,随着氧分压的升高,Si-O-Si伸缩振动峰向高波数方向移动,较高氧分压下沉积的SiO2薄膜具有较高的化学结合能,且结构和性能更稳定。     

外置式电感耦合化学气相沉积法低温制备SiO2薄膜

设计了一种外置式电感耦合等离子增强化学气相沉积装置,并利用该装置在n型硅片上低温沉积了SiO2薄膜。通过扫描电子显微镜(SEM)、傅立叶变换红外吸收谱(FTIR)等对生长的薄膜进行表征。SEM测试结果表明,利用该装置沉积的SiO2薄膜表面平整,薄膜均匀性好;根据FTIR图中Si-O峰的横向与纵向光学声子吸收峰的分析发现,沉积功率越大,薄膜越疏松;等离子体区域内不同位置沉积的薄膜均匀,能够用于大规模、大面积的工业生产。此外,为了方便地获知SiO2薄膜的厚度,我们推导出了50W的功率下,薄膜厚度随沉积温度、沉积时间变化的经验公式。     

化学溶液电沉积法制备Li2SiO3薄膜研究

利用化学溶液电沉积方法，在阴极和阳极衬底材料上都成功制备出了单相的含氧酸盐硅酸锂（Li2SiO3）薄膜。探讨了该工艺下的实验反应机理。通过X射线衍射技术（XRD）、扫描电子显微镜（SEM）分别表征研究了不同实验条件下薄膜的晶体结构和表面形貌。研究结果表明，采用化学溶液电沉积法制备的Li2SiO3薄膜具有物相结构单一，表面形貌平整致密的特点。与制备Li2SiO3的传统方法相比，这一技术具有廉价、简单、低温等特点。     

ZnO/SiO2复合薄膜的制备及其阻隔性能研究

目的为了进一步提高氧化锌(ZnO)沉积复合薄膜对氧气的阻隔能力,探索其应用于食品和药品包装材料的可行性。方法采用射频磁控溅射技术(RF),以ZnO和二氧化硅(SiO2)为靶材,在PET塑料表面同时沉积,制备ZnO/SiO2复合薄膜包装材料,并详细分析SiO2的引入对ZnO沉积膜微观结构和阻隔能力的影响,优化ZnO/SiO2的制备工艺。结果SiO2的引入,使ZnO纳米颗粒的形状由片状燕麦变成了球形,当功率密度比PSiO2/PZnO为0.67,氩气流量为20 mL/min,沉积时间为20 min,工作气压为0.5 Pa时,ZnO/SiO2复合薄膜的氧气透过率降低为0.462 mL/(m^2·d),水蒸气透过率有所增加,为0.367 g/(m^2·d)。结论引入合适比例的SiO2,可有效提升ZnO沉积层对氧气渗入的阻隔能力,但SiO2引入量过高时,会加剧纳米裂纹,对复合薄膜的阻隔能力不利。     

Wavefront control of SiO2-based ultraviolet narrow-bandpass filters prepared by plasma ion-assisted deposition

Metal oxide layers produced by plasma ion-assisted deposition are extensively used for complex optical coatings due to the availability of materials, the high packing density of films, and the smooth surfaces. Stringent optical surface figure specifications necessary for both laser optics and precision optics require film stress to be well-controlled and surface deformation to be corrected or compensated. SiO(2)- based single-cavity UV narrow-bandpass filters were prepared by plasma ion-assisted deposition. The correlation between film stress, refractive index, deposition parameters, and postdeposition annealing was established. The film stress was calculated based on interferometric surface deformation. The refractive index and film thickness were determined by means of variable angle spectroscopic ellipsometry. The center wavelength of the filters was obtained through spectral transmission measurement. The results suggest that the wavefront distortion of the multilayer coatings is dominated by the compressive stress of the SiO(2) layers and can be controlled and corrected by the amount of plasma ion momentum transfer, substrate temperature, postdeposition annealing, and stress compensation via backside SiO(2) coating. Based on the understanding of the mechanical and optical properties, the wavefront correction technique enables us to satisfy stringent surface figure specifications.     

Effect of the working gas of the ion-assisted source on the optical and mechanical properties of SiO2 films deposited by dual ion beam sputtering with Si and SiO2 as the starting materials

Silicon and fused-silica targets are used as the starting materials for depositing silicon oxide (SiO2) films. The SiO2 films are prepared by a dual ion beam sputtering deposition system with a main ion source and an ion-assisted source with different working gases. The films deposited are then examined and compared by using a visible spectrophotometer, a Fourier-transform IR spectrophotometer, an atomic force microscope, and contact angle instruments. A Twyman-Green interferometer is employed to study the film stress by phase-shift interferometry. All the SiO2 films show excellent optical properties with extra-low extinction coefficients (below 2x10(-5)) and have no water absorption. When the working gas is O2 for the ion-assisted source, the deposited SiO2 films show good properties in terms of stress and roughness and with a good molecular bonding structure order for both targets. However, SiO2 films deposited from the fused-silica target had a larger contact angle, while those deposited from the silicon target had 2.5 times the deposition rate.     

Fabrication of silica-based multilayer films with self-cleaning and antireflective properties

The silica-based multilayer films exhibiting both self-cleaning property and antireflection in the visible and near infrared regions have been deposited onto glass substrate by layer-by-layer deposition of PAH/PAA polyelectrolyte bilayers, followed by sequential deposition of PAH/SiO2 nanocomposite layers to create the nanoporous structure in the film, and finally treating with fluorosilane. To obtain the appropriate porosity and surface roughness so as to satisfy both antireflection and self-cleaning properties, the deposition of PAH/SiO2 nanocomposite layers was varied from 2 to 8 layers. Scanning electron microscopy and atomic force microscopy analysis revealed that a highly nanoporous structure was obtained from the more deposition of loosely agglomerated SiO2 nanoparticles which increased with the increased cycle of PAH/SiO2 deposition. The film consisting of 6 and 8 PAH/SiO2 layers exhibited a very low reflection of only 1-2% in the visible region and approximately 2-4% in the near infrared region, a maximum transmittance of approximately 93% in the visible region and approximately 94% in the near infrared region, and a high advancing contact angle of approximaetly 150 degrees. It is anticipated that the film which exhibited both self-cleaning and antireflection properties enables the application of the antireflection coatings under humid environments.     

TiO2和SiO2薄膜应力在线测量与研究

研究了离子能量在薄膜制备过程中对TiO2和SiO2薄膜应力的影响。用电子束蒸发的方法制备TiO2和SiO2薄膜,使用实验室自行设计制作的基于哈特曼传感器的薄膜应力仪在线监测TiO2和SiO2薄膜应力随膜厚的变化。结果表明,离子辅助沉积的TiO2薄膜张应力值要比传统工艺低40 MPa,并且随着离子能量的增加,薄膜逐渐由张应力变为压应力,薄膜的最大折射率为2.56;而离子辅助的溅射效应在制备SiO2薄膜时比较明显,传统工艺制备的SiO2薄膜表现为压应力,而用离子辅助的方法制备的SiO2薄膜表现为张应力,并且随着离子能量的增加,薄膜变得疏松,折射率逐渐降低。     

Optical properties of electrochemically deposited ZnO thin films on colloidal crystal film of SiO2 microspheres

The optical properties of electrochemically deposited ZnO thin films on colloidal crystal film of SiO2 microspheres structures were studied. Colloidal crystal film of SiO2 microspheres were self-assembled by evaporation using SiO2 in solution at a constant 0.1 wt%. ZnO in thin films was then electrochemically deposited on to colloidal crystal film of SiO2 microspheres. During electrochemical deposition, the content of Zn(NO3)2 x 6H2O in solution was 5 wt%, and the process's conditions were varied between of 2-4 V and 30-120 s at room temperature, with subsequent heat-treatment between 200 and 400 degrees C. A smooth surface and uniform thickness of 1.8 microm were obtained at 3 V for 90 s. The highest PL peak intensity was obtained in the ZnO thin film heat-treated at 400 degrees C. The double layered ZnO/SiO2 colloidal crystals showed clearly better emission properties than the SiO2/ZnO and ZnO structures.     

基片温度对磁控溅射沉积二氧化硅的影响

本文详细地研究了基片温度对磁控溅射沉积二氧化硅的影响,随着基片温度的增加,溅射沉积速率下降明显,薄膜的折射率也出现上升趋势,薄膜也由低温时的疏松粗糙发展为致密光滑.250℃时的溅射沉积速率仅为室温时的1/3,由此,针对间歇式在大面积玻璃上沉积二氧化硅薄膜,我们采取了沉积完ITO薄膜后,先快速降温,再沉积二氧化硅的工艺.     

Mechanical characteristics of optical coatings prepared by various techniques: a comparative study

Good performance of optical coatings depends on the appropriate combination of optical and mechanical properties. Therefore, successful applications require good understanding of the relationship between optical microstructural and mechanical characteristics and film stability. In addition, there is a lack of standard mechanical tests that allow one to compare film properties measured in different laboratories. We give an overview of the methodology of mechanical measurements suitable for optical coatings; this includes depth-sensing indentation, scratch resistance, friction, abrasion and wear testing, and stress and adhesion evaluation. We used the techniques mentioned above in the same laboratory to systematically compare the mechanical behavior of frequently used high- and low-index materials, namely, TiO2, Ta2O5, and SiO2, prepared by different complementary techniques. They include ion-beam-assisted deposition by electron-beam evaporation, magnetron sputtering, dual-ion-beam sputtering, plasma-enhanced chemical-vapor deposition, and filtered cathodic arc deposition. The mechanical properties are correlated with the film microstructure that is inherently related to energetic conditions during film growth.     

Elastic and plastic relaxation of densified SiO2 films

Ion- and plasma-assisted deposition has been extensively used for the fabrication of high-performance optical films with dense and smooth microstructures that are essential for applications such as low-loss and environmentally stable optics. SiO(2) is a well-known amorphous material suitable for energetic deposition. SiO(2) single layers and SiO(2)-based single-cavity narrow-bandpass filters were prepared by plasma-ion-assisted deposition. The refractive index and film thickness were determined by variable-angle spectroscopic ellipsometry. The high compressive stress of the densified film was correlated to increased packing density. The center wavelength shift of the narrow-bandpass filters as a function of sample-temperature as well as high-temperature annealing was determined via spectral transmission measurement. Structural relaxation of the densified SiO(2) films was observed from the variation of the refractive index and physical thickness for the single layers and the center wavelength shift for the narrow-bandpass filters, suggesting elastic and plastic deformation of the densified films corresponding to a reversible and an irreversible center wavelength shift, respectively.     

蓝宝石衬底上制备SiO2薄膜的研究

采用射频磁控反应溅射法,以高纯Si为靶材,高纯O2为反应气体,成功地在蓝宝石基片上制备出了二氧化硅(SiO2)薄膜,并对薄膜的沉积速率、成分、结构及红外光学性能进行了研究.结果表明,制备的SiO2薄膜与蓝宝石衬底结合牢固;和其它镀膜技术相比,射频磁控反应溅射法可以在较低的温度下制备出SiO2薄膜;制备出的SiO2薄膜在3～5μm波段对蓝宝石衬底有明显的增透效果.