Oxidation of evaporated porous silicon rugate filters

Rugate filters are thin-film optical interference coatings with sinusoidal variation of the refractive index. Several of these filters were fabricated with glancing angle deposition, which exploits atomic competition during growth to create nanoporous materials with controllable effective refractive index. This method enables the fabrication of devices with almost arbitrary refractive index profiles varying between the ambient, 1.0, and the index of the film material, in this case silicon with an index of 4.0 (at 600 nm). As these filters are inherently porous, oxidation of the silicon can occur throughout the device layer, and here we study the intentional oxidation of silicon filters by high-temperature reaction with gaseous oxygen. We find that a significant portion of the silicon filter oxidizes in approximately 10 min when heated to 600 degrees C-650 degrees C in an oxygen environment; oxidation then continues slowly over several hours. The presence of water vapor has little apparent effect on the oxidation reaction, and attempts to oxidize with ozone at room temperature were unsuccessful. As silicon filters oxidize to become silica, spectral blueshifts and increased short-wavelength transmittance are observed. Measured and calculated transmittance spectra generally agree, although the lack of absorption and dispersion in the theoretical model limits detailed comparison.     

Enhancement in broadband and quasi-omnidirectional antireflection of nanopillar arrays by ion milling

A new technique is developed to fabricate biomimetic antireflection coatings (ARCs). This technique combines a bottom-up fabrication approach (glancing angle deposition, or GLAD) with a top-down engineering process (ion milling). The GLAD technique is first utilized to produce nanopillar arrays (NPAs) with broadened structures, which are subsequently transformed into biomimetic tapered geometries by means of post-deposition ion milling. This structure transformation, due to milling-induced mass redistribution, remarkably decreases reflection over a wide wavelength range (300-1700 nm) and field of view (angle of incidence < 60° with respect to the substrate normal). The milling-induced antireflection enhancement has been demonstrated in the NPAs made of Si, SiO(x) and TiO(2), illustrating that this integrated technique is readily adapted to a wide variety of materials. Good agreement between simulation and experiment indicates that the enhanced antireflection performance is ascribed to a smoother refractive index transition from the substrate to the air, which improves the impedance match and reduces reflection losses. Additionally, ion bombardment tends to alter the stoichiometry and diminish the crystallographic structure of the NPA materials. The broadband and quasi-omnidirectional antireflection observed establishes the strong competitiveness of this technique with the methods previously reported.     

A study of silicon oxynitride film prepared by ion beam assisted deposition

A SOI-based optoelectronic device needs a high-quality antireflection coating on both faces of the device to minimize the optical reflectance from the face. In this work amorphous silicon oxynitride films were deposited on silicon substrates by ion beam assisted deposition (IBAD). The main purpose was to use silicon oxynitride film as single layer anti-reflection coating for SOI-based optoelectronic devices. This application is primarily based on the ability to tune the silicon oxynitride optical functions to the optimal values by changing deposition parameters. The chemical information was measured by X-ray photoelectron spectroscopy (XPS). Spectroscopic ellipsometry (SE) was applied to measure the refractive index and thickness. Single-side polished silicon substrate that was coated with silicon oxynitride film exhibited low reflectance. Double-side polished silicon substrate that was coated with silicon oxynitride film exhibited high transmittance. In addition, the Fresnel losses could be reduced to 0.08 dB by depositing silicon oxynitride films onto double-side polished silicon substrates. The results suggested silicon oxynitride film was a very attractive single layer anti-reflection coating for SOI-based optoelectronic device.     

In situ and air index measurements: influence of the deposition parameters on the shift of TiO2/SiO2 Fabry-Perot filters

We measure the refractive index of thin films of TiO2 and SiO2 for given deposition parameters. Two complementary methods are used. The first is a postdeposition technique which uses the measurements of reflectance and transmittance in air. The second, in contrast, makes use of in situ measurements (under vacuum and during the actual deposition of the layer). The differences between the values deduced from the two methods can be explained by the amount of atmospheric moisture adsorbed by films. One tries to minimize these shifts for the two materials by choosing deposition parameters. The difficulties come from the absorption losses which must be as small as possible. We use the measured refractive indices of individual layers to give good numerical prediction of the wavelength shift (observed during the admittance of air after deposition in the vacuum chamber) of the transmittance peak of multidielectric Fabry-Perot filters.     

Universal antireflection coatings for substrates for the visible spectral region

It is possible to design normal-incidence antireflection coatings that reduce the reflectance of any substrate with a refractive index that lies in the range of 1.48 to 1.75. The performance of such coatings depends on the width of the spectral region over which the reflectance is to be suppressed, on the coating materials used for their construction, and on the overall optical thickness of the layer system. For example, the calculated average spectral reflectance of a set of six different substrates with refractive indices 1.48, 1.55, 1.60, 1.65, 1.70, and 1.75, when coated with a 0.56-μm-thick, eight-layer antireflection coating designed for the 0.40-0.80-μm spectral region, was 0.34%. This is higher than the average reflectance that is attainable with a conventional antireflection coating of similar optical thicknesses designed for a particular refractive index. However, it is an acceptable value for most applications. With the universal type of antireflection coating described, it is thus possible to coat a number of different refractive-index substrates in one deposition run, and this can result in considerable cost and time savings.     

PEM控制中频孪生反应磁控溅射沉积TiO2薄膜的研究

在中频孪生靶反应磁控溅射实验装置上,用PEM控制沉积TiO2薄膜,实验了靶基距、电流与沉积速率的关系。实验得出,靶基距为112 mm时沉积速率最大,沉积速率与电流基本成线性比例关系。在溅射电流30 A,靶基距112 mm,设置点2.5时,测量了基片随时间的温升变化。然后以自然温升的单晶硅为基片,实验研究了设置点对TiO2薄膜晶体结构、折射率的影响。实验结果表明,设置点越高溅射沉积的薄膜金红石相越多,折射率也越高。     

Narrow line-width filters based on rugate structure and antireflection coating

Filters that have high transmittance over the passband region of the reflectance spectrum are designed by combining rugate structures and antireflection (AR) coatings. It is found that, under certain conditions, the refractive index of the substrate could be “converted” to the air-side refractive index of the graded-refractive-index coating. A method for the fabrication of graded-index coatings by rapidly alternating deposition of low (SiO₂) and high (Nb₂O₅) refractive index materials is introduced, and this technology was used to fabricate a rugate structure. An AR coating with a refractive index of 1.23 was grown onto the rugate structure by glancing angle deposition technology. Optical measurements of the combined structure show excellent transmittances over the wavelength regions around the reflection band and high reflectances in the stopband.     

Deposition and spectral performance of an inhomogeneous broadband wide-angular antireflective coating

Gradient index coatings and optical filters are a challenge for fabrication. In a round-robin experiment, basically the same hybrid antireflection coating for the visible spectral region, combining homogeneous refractive index layers of pure materials and linear gradient refractive index layers of material mixtures, has been deposited. The experiment involved three different deposition techniques: electron-beam evaporation, ion-beam sputtering, and radio frequency magnetron sputtering. The material combinations used by these techniques were Nb(2)O(5)/SiO(2), TiO(2)/SiO(2), and Ta(2)O(5)/SiO(2), respectively. The spectral performances of samples coated on one side and on both sides have been compared to the corresponding theoretical spectra of the designed profile. Also, the reproducibility of results for each process is verified. Finally, it is shown that ion-beam sputtering gave the best results in terms of deviation from the theoretical performance and reproducibility.     

Characterization of silicon oxynitride thin films deposited by electron beam physical vapor deposition technique

Thin films of silicon oxynitride (SiO_xN_y) were deposited successfully on silicon wafer substrates using electron beam physical vapor deposition (EB-PVD) technique by varying the substrate temperature (T=100–450 °C) and deposition time (t=0.5–2.5 min). The films were characterized by UV–Visible and X-ray photoelectron spectroscopy (XPS), Tally step measurement and Ellipsometry. The minimum reflectivity R=1.72% is obtained for the films deposited under the conditions of T=350 °C, t=1.5 min at λ=548 nm. Further, the characterization results revealed that the refractive index (RI) of the films increases with increase in the substrate temperature due to increase in silicon nitride content. The refractive index and the thickness of the films were found to be in the range of n=1.72–1.90 and d=40–138 nm, respectively. The values n=1.88 and d=79 nm observed corresponding to the minimum reflectivity R=1.72% satisfy the condition of near quarter wavelength single layer antireflection coating. Thus, the above films might have the tremendous potential for antireflective coating applications.     

用ECRCVD方法制备优质氮化硅钝化膜

利用电子回旋共振等离子体化学气相沉积(ECR—CVD)技术，以SiH4和N2为反应气体进行了氮化硅钝化薄膜的低温沉积技术的研究。采用原子力显微镜、傅立叶变换红外光谱和椭圆偏振光检测等技术对薄膜的表面形貌、结构、厚度和折射率等性质进行了测量。结果表明，采用ECR—CVD技术能够在较低的衬底温度条件下以较高的沉积速率制备厚度均匀的氮化硅薄膜，薄膜中H含量很低。薄膜沉积速率随微波功率和混合气体中硅烷比例的增加而增大。折射率随微波功率的增大而减小，随混合气体中硅炕比例的增大而增大。在相同气体混合比和微波功率条件下，较高衬底温度条件下制备的薄膜折射率较大。     

Silica nanofilms deposited by atmospheric pressure plasma liquid deposition

Silica coatings were deposited onto pure silicon surfaces by a deposition technique known as atmospheric pressure plasma liquid deposition using liquid tetraethylorthosilicate (TEOS) as a precursor. Deposition parameters were varied, including power, TEOS flow rate, helium flow rate, and substrate distance, in order to assess their influence on the growth rates and refractive index as well as the formation of surface particulates and organic content of the coatings. Growth rates were accurately controlled in the range of 0.5 nm s^− 1 to 7.2 nm s^− 1, with thin-films having refractive indices ranging from 1.1 to 1.4, indicative of layers with different levels of porosity. The results suggest that, with careful selection of deposition parameters, this (atmospheric pressure) plasma-based deposition technique could be used to achieve coherent, particulate free, smooth dense inorganic silica coatings.     

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.     

Optical properties of solution-processable semiconducting TiOx thin films for solar cell and other applications

The optical properties of solution-processable semiconducting titanium suboxide (TiOx) thin films were investigated as a function of wavelength (350-800 nm) using ellipsometric and optical reflection technique. The variation of refractive index under different thermal annealing conditions (room temperature to 900 °C) was studied. The increase in refractive index with high-temperature thermal annealing process was observed, allowing the opportunity to obtain refractive index values from 1.77 to 2.57 at a wavelength of 600 nm. The x-ray diffraction and atomic force microscopy studies indicate that the index variation is due to the TiOx phase, density, and morphology changes under thermal annealing. The TiOx thin films have applications in organic and inorganic solar cells as well as other optical and photonic devices. We show that TiOx thin films can be used as an effective antireflection layer for Si solar cells.     

Low refractive index silicon oxide coatings at room temperature using atmospheric-pressure very high-frequency plasma

Low refractive index silicon oxide films were deposited using atmospheric-pressure He/SiH₄/CO₂ plasma excited by a 150-MHz very high-frequency power. Significant increase in deposition rate at room temperature could prevent the formation of dense SiO₂ network, decreasing refractive index of the resulting film effectively. As a result, a silicon oxide film with the lowest refractive index, n = 1.24 at 632.8 nm, was obtained with a very high deposition rate of 235 nm/s. The reflectance and transmittance spectra showed that the low refractive index film functioned as a quarter-wave anti-reflection coating of a glass substrate.     

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.     

Optical properties of hydrogenated hard carbon thin films

Hydrogenated amorphous carbon (a-C:H) films were deposited onto glass, silicon and germanium substrates. The films are transparent in the IR and are extremely hard (Mohs' hardness of about 8). The a-C:H coatings were prepared in an r.f.-excited discharge sustained by various hydrocarbon gases.The thickness, density, refractive index (at 0.3 μm and 2–10 μm) and relative hydrogen content were determined. Variations in the IR refractive index and the relative hydrogen content could be correlated with the deposition conditions. With a refractive index of approximately 2 a-C:H is an ideal antireflection coating for germanium (n = 4).Laser calorimetric measurements of optical absorption at 10.6 μm give a loss as low as 3% for a coating 1.3 μm thick on germanium (λ/4 for n = 2 at 10.6 μm).     

锗掺杂类金刚石薄膜特性研究

为了降低类金刚石(DLC)薄膜的应力,使用脉冲真空电弧离子镀(PVAD)和电子束热蒸发相结合的复合沉积技术,在Si基底上制备了一系列不同锗含量(原子百分比)的Ge-DLC薄膜样片,研究了锗含量对DLC薄膜光学特性和力学特性的影响。研究结果表明:在1~5μm波段,当锗掺杂含量小于25%时,对DLC薄膜光学常数的影响不大;随着Ge含量的增加,DLC薄膜的折射率和消光系数都略微增大。随着DLC薄膜中Ge含量的增加,薄膜的内应力和硬度均有所降低。当DLC薄膜中Ge含量约为8%时,Ge-DLC薄膜的内应力从6.3降至3.0 GPa,而硬度仅从3875减小为3640 kgf/mm2,几乎保持不变。硅基底上单面沉积Ge的含量为8%的DLC薄膜在红外3~5μm波段的透过率峰值约为63.15%。     

LOW FREQUENCY GLOW DISCHARGE HYDROGENATED AMORPHOUS SILICON CARBIDE FILMS

Hydrogenated amorphous Si_xC_1-x:H films with various compositions were prepared by low frequency (110 kHz) glow discharge decomposition of a silane and methane mixture diluted by helium. The deposition rate, the composition, the structure and the refractive index of the films were studied using SEM, AES and IB analyses. Only the deposition rate was found to be influenced by the position of the silicon substrate in the reactor. From infrared analyses we estimate that the structure of the films is a tetrahedral network where carbon atoms are randomly replaced by silicon atoms and where only one single hydrogen is bound to silicon. The rather dense and inorganic character of these films is confirmed by the high values of their refractive index ranging from 2.1 for x=0 to 3.4 for x=1.     

类金刚石薄膜光学特性的椭偏法研究

本文采用脉冲电弧离子镀的方法,在p型硅上沉积类金刚石薄膜,用椭偏法测试薄膜的光学常数.根据沉积方法的特点,建立一个四层结构的膜系,并由每一层的吸收情况合理选择色散关系;结合透过率的测试结果,利用光度法给测出薄膜折射率和厚度的估计值,作为椭偏法拟合的初值,拟合效果良好,得到薄膜的折射率、消光系数和几何厚度.     

Optimization of PECVD silicon oxynitride films for anti-reflection coating

In this work, amorphous silicon oxynitride films were deposited on silicon substrates by plasma-enhanced chemical vapor deposition (PECVD). The main purpose was to use silicon oxynitride film as a single-layer anti-reflection coating for Si-based optoelectronic devices. The chemical information was measured by infrared spectroscopy. Surface and cross-section morphology was determined by a scanning electron microscope. Spectroscopic ellipsometry (SE) was applied to measure the refractive index, extinction coefficient and thickness. The results of SE presented the refractive indices varied in the range of 1.83-1.92 by altering SiH₄/NH₃ ratio. One-side polished silicon substrate coated with silicon oxynitride film exhibited low reflectance, and two-side polished silicon substrate coated with silicon oxynitride film exhibited high transmittance. The results suggested that silicon oxynitride film was a very attractive single-layer anti-reflection coating.