Structural characterization of oxide layers thermally grown on 3C-SiC films

The oxidation of 3C-SiC films deposited on off-oriented Si(001) substrates by reactive magnetron sputtering has been studied. The oxidation was carried out using dry conditions at a temperature of 1200°C. The composition of the oxide layer was investigated by Auger electron spectroscopy (AES). The oxide layer was found to contain no C except for the region very close to the interface, and the stoichiometry was found to be close to that of SiO₂. Cross-sectional transmis-sion electron microscopy (XTEM) showed the oxide layer to be completely amorphous, dense, and homogeneous with a uniform thickness. High-resolution XTEM imaging showed an atomically sharp SiO₂/SiC interface.     

Use of electron cyclotron resonance plasmas to prepare CdZnTe (211)B substrates for HgCdTe molecular beam epitaxy

Without any additional preparation, Cd_1−yZn_yTe (211)B (y∼3.5%) wafers were cleaned by exposure to an electron cyclotron resonance (ECR) Ar/H₂ plasma and used as substrates for HgCdTe molecular beam epitaxy. Auger electron spectra were taken from as-received wafers, conventionally prepared wafers (bromine: methanol etching, followed by heating to 330–340°C), and wafers prepared under a variety of ECR process conditions. Surfaces of as-received wafers contained ∼1.5 monolayers of contaminants (oxygen, carbon, and chlorine). Conventionally prepared wafers had ∼1/4 monolayer of carbon contamination, as well as excess tellurium and/or excess zinc depending on the heating process used. Auger spectra from plasma-treated CdZnTe wafers showed surfaces free from contamination, with the expected stoichiometry. Stoichiometry and surface cleanliness were insensitive to the duration of plasma exposure (2–20 s) and to changes in radio frequency input power (20–100 W). Reflection high energy electron diffraction patterns were streaked indicating microscopically smooth and ordered surfaces. The smoothness of plasma-etched CdZnTe wafers was further confirmed ex situ using interferometric microscopy. Surface roughness values of ∼0.4 nm were measured. Characteristics of HgCdTe epilayers deposited on wafers prepared with plasma and conventional etching were found to be comparable. For these epilayers, etch pit densities on the order of 10⁵ cm⁻² have been achieved. ECR Ar/H₂ plasma cleaning is now utilized at Night Vision and Electronic Sensors Directorate as the baseline CdZnTe surface preparation technique.     

溅射沉积AlN薄膜结构与基片种类的关系

采用高真空直流磁控反应溅射成功地在５种基片上制备出多晶择优取向的ＡＩＮ薄膜。结果表明,５种基片均可生长（１００）面掺优取向的ＡＩＮ薄膜,并且具有良好的纵向组成均匀性,表面粗造度小,晶粒均匀致密。在金属电极和Ｓｉ片上沉积的ＡＩＮ薄膜结晶度、取向性、衍射强度差别较小,两者的结构均优于在盖玻片上的沉积的ＡＩＮ薄膜。     

Ion Beam Analysis of Amorphous and Nanocrystalline Group III-V Nitride and ZnO Thin Films

The ion beam analysis (IBA) techniques of Rutherford backscattering spectrometry (RBS), elastic recoil detection analysis (ERDA), nuclear reaction analysis (NRA), and particle-induced x-ray emission (PIXE) have been used to quantitatively determine composition, uniformity, impurity, and elemental depth profiles of major, minor, and trace elements of group III-V nitride and zinc oxide (ZnO) thin films prepared by various growth techniques. The IBA revealed that an amorphous GaN film prepared by ion beam assisted deposition (IBAD) has large variations in film thickness and composition coupled with typically 10–20% oxygen that was found to be essential to stabilize their amorphous structure. The IBA characterization of plasma-assisted molecular beam epitaxy (PAMBE) grown GaN, InN, and InCrN films revealed composition, impurity, and uniformity information of the films. The IBA of ZnO films prepared by radio frequency (RF) sputtering showed that the Zn/O ratio often varied significantly over the film thickness. Hydrogen was found to be a major impurity in the films with around one present in the as-deposited ZnO films. It is clearly shown that the nondestructive, quantitative, and rapid IBA measurements are very useful to develop and optimize growth protocols in respect to film thickness, stoichiometry, and especially in regard to hydrogen and oxygen impurities for group III-V nitride and ZnO thin films prepared by various growth techniques.     

改善玻璃衬底上ZnO薄膜特性的方法

利用磁控溅射法在玻璃衬底上淀积铝掺杂氧化锌(AZO)薄膜作为缓冲层,在其上制备了ZnO薄膜。重点研究了AZO薄膜作为缓冲层对玻璃衬底上ZnO薄膜特性的影响。扫描电子显微镜(SEM)图像和X射线衍射(XRD)图谱分析结果表明,玻璃衬底上加入厚度为1μm的AZO缓冲层后,提高了衬底材料和ZnO薄膜之间的晶格匹配程度,有助于增大ZnO薄膜晶粒尺寸,提高其(002)取向择优生长特性、薄膜结晶特性及晶格结构完整性。室温下的透射光谱结果表明玻璃/AZO和玻璃衬底上ZnO薄膜的透光特性没有显著不同。光致发光(PL)谱研究结果表明AZO缓冲层可以有效阻止衬底表面硅原子从ZnO薄膜中"俘获"氧原子,减少ZnO薄膜中的缺陷,改善ZnO薄膜的结晶质量。     

Low-temperature metal-organic chemical vapor deposition (LTMOCVD) of device-quality copper films for microelectronic applications

Copper films for potential use in multilevel metallization in ULSIC’s were produced by low temperature (250–350° C) metal-organic chemical vapor deposition (LTMOCVD) in atmospheres of pure H₂ or mixture Ar/H₂ from the β-diketonate precursor bis(1,1,1,5,5,5-hexafluoroacetylacetonato) copper(ll), Cu(hfa)₂. The films were analyzed by x-ray diffraction (XRD), Rutherford backscattering (RBS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and energy-dispersive x-ray spectroscopy (EDXS). The results of these studies showed that the films were uniform, continuous, adherent and highly pure—oxygen and carbon contents were below the detection limits of AES. Four point resistivity measurements showed that the copper films had very low resistivity, as low as 1.9 μΩcm for the films deposited in pure hydrogen atmosphere. Our preliminary results seem to indicate that LTMOCVD is a very attractive technique for copper multilevel metallizations.     

ITO薄膜厚度和含氧量对其结构与性能的影响

在玻璃衬底上用直流磁控溅射的方法镀制ITO透明半导体膜,采用X射线衍射技术分析了膜层晶体结构与薄膜厚度和氧含量的关系,并测量了薄膜电阻率及透光率分别随膜厚和氧含量的变化情况。以低氧氩流量比(1/40)并控制膜厚在70nm以上进行镀膜,获得了结晶性好、电阻率低且透光率高的ITO透明半导体薄膜,所镀制的ITO膜电阻率降到1.8×10–4?·cm,可见光透光率达80%以上。     

Effect of Al Nanoparticles on the Microstructure,Electrical, and Optical Properties of AZO/Al/AZO Trilayer Thin Film

In this work, designed growth of aluminum (Al)/aluminum-doped zinc oxide (AZO), AZO/Al/AZO, and AZO/Al multilayer electrodes by radiofrequency (RF) magnetron sputtering on glass substrates was studied. The microstructures, optical properties, and electrical characteristics of the multilayer electrode thin films were analyzed, their structural denseness and thickness were observed by field-emission scanning electron microscopy (FE-SEM), and their crystal orientation was identified by x-ray diffraction (XRD). The resistivity and transmittance of the films were measured by four-point probe and UV–Vis–NIR spectrophotometer, respectively. The resistivity of the AZO/Al/AZO multilayer electrode thin film was 1.55 Ω cm. The average transmittance of the AZO/Al/AZO thin film over wavelengths from 400 nm to 800 nm was much better than that of other thin films, since Al nanoparticles distribute in the AZO thin film during the sputtering process, as observed by high-resolution transmission electron microscopy (HRTEM). In addition, the figure of merit of the AZO/Al/AZO trilayer film was much larger than those of the other structures.     

Characterization of sputtered nano-crystalline zirconium carbide as a diffusion barrier for Cu metallization

Zirconium carbide (ZrC) films were grown on Si (100) substrates using magnetron sputtering where the growth temperature (T_s) was varied from 25°C to 290°C. The microstructure and resistivity of the as-deposited ZrC films were examined. The results reveal that nano-crystalline ZrC films with grain size less than 5 nm were fabricated only at 29°C, which can be explained by a repeated nucleation mechanism. For thermal stability characterization, the stacked structure of Cu/ZrC/Si was subsequently subject to thermal treatments at temperatures from 300°C to 900°C for 30 min in a vacuum tube. The stacked samples were shown to be thermally stable up to about 800°C from Auger electron spectroscopy (AES) and x-ray diffraction (XRD). The diffusion coefficient and activation energy of Cu and Si in the ZrC barrier were also derived. It indicated that Si has a lower activation energy than Cu resulting in faster diffusion. The device completely fails at 900°C, and the mechanism is discussed in this paper.     

Physical properties of SnS thin films fabricated by hot wall deposition

The dependence of the microstructure and optical properties of SnS thin films fabricated by hot wall deposition onto glass substrates on the deposition conditions is studied. Phase and elemental composition, surface morphology, and transmission spectra of the obtained films are investigated within the wavelength range 400–2500 nm. The single-phase films feature near-stoichiometric elemental composition and a high degree of preferential orientation in the (040) plane. The optical band gap for direct transitions is 1.07–1.27 eV, depending on film thickness.     

Degenerate cadmium oxide films for electronic devices

Highly conducting and transparent cadmium oxide films have been deposited on Corning 7059 glass substrates by ion-beam sputtering and by spray pyrolysis. The electrical and optical properties of CdO films prepared by the two techniques are similar. Typical films of 0.5 μm thickness have electrical resistivities of (2–5) × 10^-3 ohm-cm, carrier concentrations of approximately 10²⁰ cm^-3, and an optical transmission of higher than 70% in the wavelength range of 600–900 nm. An optical bandgap of 2.4–2.42 eV was deduced from the optical transmission data.     

Tensile properties of aluminum/alumina multi-layered thin films

Thin, free standing aluminum and alumina films were produced by physical vapor deposition and tensile properties were measured. Young’s modulus of the aluminum was microstructure insensitive, but the plastic behavior was very structure sensitive. The natural surface oxide of the aluminum had no apparent affect on the measured value ofYoung’s modulus. The alumina films showed true brittle behavior, but Young’s modulus was lower than bulk. Impurities residing at the grain boundaries were observed in the aluminum films using transverse Auger electron spectroscopy (AES). The films were well characterized using AES, transmission electron microscopy, Rutherford backscattering spectroscopy, and secondary electron microscopy. Well characterized, thin three-layered aluminum/alumina compositionally modulated films were produced by alternate depositions and tensile properties were measured. Young’s modulus was found to be less than a weighted thickness average of Young’s modulus of the individual constituents. Otherwise, the mechanical measurements yielded typical bulk behavior.     

直流磁控溅射ZnO薄膜的结构特性

通过改变工作气压、溅射电流、氩氧比等工艺参数,较为系统地探索了用反应式直流磁控溅射法制备ＺｎＯ薄膜的工艺条件,并采用ＸＲＤ和ＡＥＳ对这些薄膜的结构特性进行测试分析,成功地得到了具有ｃ轴择优取向、结晶度高的ＺｎＯ薄膜。     

Analysis of the stress and interfacial reactions in Pt/Ti/SiO2/Si for use with ferroelectric thin films

The microstructure of the Pt/Ti/SiO₂/Si structure has been investigated by scanning and transmission electron microscopy. Pt films of 100 nm thickness deposited by sputtering or evaporation onto unheated substrates gave complete coverage of the underlying Ti layer and showed a granular and faceted structure with grains ∼20 nm in diameter. They did not exhibit hillocks or surface TiO_x formation. X-ray diffraction was used to examine the film stress through use of the sin²ψ method with bulk values for the elastic constants (v=0.39, E=162 GPa). The as-deposited sputtered film had a compressive stress of ∼540 MPa, while the evaporated films had tensile stresses of ∼630 MPa. The films then received a 400°C rapid thermal anneal (RTA) for 90 s and a subsequent RTA of 650°C for 30s. Further investigation of the film stresses and microstructure were made after each annealing step. After the low temperature anneal, the film stress for the sputtered film became tensile. Plan-view sections examined by transmission electron microscopy (TEM) showed that the as-deposited sputtered films were dense but became porous after annealing. Initially, the evaporated films had a less dense microstructure, but were more stable with annealing. Little change in the stress for the evaporated film was observed after this initial low temperature annealing step. Additional annealing of the evaporated and sputtered samples caused complete consumption of the Ti layer including some TiO_x formation from the underlying SiO₂ layer and marked interaction with the Pt; however, little change in the stress was found. The surface of the Pt film revealed larger grains, but otherwise remained unaffected. The underlying phase changes were minimized once the Ti layer had reacted with the Pt. Due to the ratio of the layers, Pt:Ti of 2:1, the surface of the Pt was unaffected.     

Structural characterization of DC magnetron-sputtered TiO2 thin films using XRD and Raman scattering studies

Titanium dioxide films have been deposited using DC magnetron sputtering technique onto well-cleaned p-silicon substrates at an oxygen partial pressure of 7×10^–5 mbar and at a sputtering pressure (Ar+O₂) of 1×10^–3 mbar. The deposited films were calcinated at 673 and 773 K. The composition of the films as analyzed using Auger electron spectroscopy reveals the stoichiometry with an O and Ti ratio 2.08. The influence of post-deposition annealing at 673 and 773 K on the structural properties of the titanium dioxide thin films have been studied using XRD and Raman scattering. The structure of the films deposited at the ambient was found to be amorphous and the films annealed at temperature 673 K and above were crystalline with anatase structure. The lattice constants, grain size, microstrain and the dislocation density of the film are calculated and correlated with annealing temperature. The Raman scattering study was performed on the as-deposited and annealed samples and the existence of Raman active modes A_1g, B_1g and E_g corresponding to the Raman shifts are studied and reported. The improvement of crystallinity of the TiO₂ films was also studied using Raman scattering studies.     

Electron cyclotron resonance plasma preparation of CdZnTe (211)B surfaces for HgCdTe molecular beam epitaxy

CdZnTe wafers were inserted into a multi-chamber processing facility without prior preparation, cleaned by exposure to an electron cyclotron resonance Ar/H₂ plasma, and used as substrates for molecular beam epitaxy of HgCdTe. Changes induced in the wafer near-surface region during the cleaning step were monitored using in situ spectroscopic ellipsometry. Ellipsometric data were subsequently modeled to provide the time evolution of the thickness of a native overlayer. Auger electron spectra were consistent with surfaces free of residual contamination and which had the stoichiometry of the underlying bulk. Surface roughness values of 0.4 nm were obtained ex situ using interferometric microscopy. Electron diffraction patterns of plasma prepared wafers heated to 185°C (the temperature required for HgCdTe molecular beam epitaxy) were streaked. Structural and electrical characteristics of epilayers grown on these substrates were found to be comparable to those deposited on wafers prepared using a conventional wet chemical process. This demonstrates an important step in an all-vacuum approach to HgCdTe detector fabrication.     

Si基GaN薄膜的制备方法及结构表征

分别采用射频磁控溅射、热壁化学气相沉积(CVD)、电泳沉积法制备GaN薄膜。利用扫描电镜(SEM)、荧光光谱仪对样品进行结构、形貌和发光特性的分析比较。射频磁控溅射方法中,把SiC中间层沉淀到Si衬底上,目的是为了缓冲由GaN外延层和Si衬底的晶格失配造成的应力。结果证实了SiC中间层提高了GaN薄膜的质量。热壁化学气相沉积法制备GaN晶体膜时,选择H2作反应气体兼载体,有利于GaN膜的形成。电泳沉积法显示所得样品为六方纤锌矿结构的GaN多晶薄膜。结果表明:溅射法制备的GaN薄膜结晶效果好;CVD法制备时GaN薄膜应用范围广;电泳沉积法操作方便、简单易行。     

Investigation into Texture,Preferential Orientation,and Optical Properties of Zinc Oxide Nanopolycrystalline Thin Films Deposited by the Sol–Gel Technique on Different Substrates

ZnO nanopolycrystalline thin films were deposited by the sol–gel technique on glass and silicon, and compared systematically via atomic force microscopy, scanning electron microscopy, x-ray diffraction, UV–Vis spectrophotometry, and fluorescence spectrophotometry. The thickness of the ZnO films was measured by ellipsometric microscopy. A higher preheating temperature was needed to obtain films with a strong preferential orientation. The optimal annealing temperatures for c-axis films on glass and silicon substrates were 525°C and 750°C, respectively. The relative intensity of the blue–green emission peak tends to increase with the annealing temperature. When the film is annealed in N₂, the transmittance of the film reduces while the intensity of the blue–green emission increases.     

Microstructure and enhanced morphology of planar nonpolar m-plane GaN grown by hydride vapor phase epitaxy

Nonpolar ( ) m-plane gallium nitride has been grown heteroepitaxially on (100) γ-LiAlO₂ by several groups. Previous attempts to grow m-plane GaN by hydride vapor phase epitaxy (HVPE) yielded films unsuitable for subsequent device regrowth because of the high densities of faceted voids intersecting the films’ free surfaces. We report here on the growth of planar m-plane GaN films on (100) γ-LiAlO₂ and elimination of bulk and surface defects. The morphology achieved is smooth enough to allow for fabrication of m-plane GaN templates and free-standing substrates for nonpolar device regrowth. The GaN films were grown in a horizontal HVPE reactor at 860–890°C. Growth rates ranged from 30 μm/h to 240 μm/h, yielding free-standing films up to 250-μm thickness. The m-plane GaN films were optically specular and mirror-like, with undulations having 50–200-nm peak-to-valley heights over millimeter length scales. Atomic force microscopy revealed a striated surface morphology, similar to that observed in m-plane GaN films grown by molecular beam epitaxy (MBE). Root-mean-square (RMS) roughness was 0.636 nm over 25-μm² areas. Transmission electron microscopy (TEM) was performed on the m-plane GaN films to quantify microstructural defect densities. Basal-plane stacking faults of 1×10⁵ cm⁻¹ were observed, while 4×10⁹ cm⁻² threading dislocations were observed in the g=0002 diffraction condition.     

Effects of annealing temperature on the photoluminescence of RF sputtered Barium titanate thin films

BaTiO₃ thin films were deposited onto quartz substrates by an RF magnetron sputtering method. The films deposited at room temperature and annealed at 773–1173 K were characterized using X-ray diffraction (XRD)Scanning electron microscopy (SEM), UV–vis spectroscopy and Photoluminescence spectroscopy (PL). X-ray diffraction studies revealed that the film is amorphous in nature at 773 K and that the crystallinity increases with increase in annealing temperature. The average crystallite size of the films increased from 13–18 nm and the optical band gap decreased in the range of 4.33–3.43 eV, with increase in annealing temperature. The films exhibited good adherence to the substrates and the SEM images showed smooth surface morphology. Energy dispersive X-ray (EDX) analysis confirmed the presence of barium, titanium and oxygen in the film. The red-shifts of excitonic UV emission peaks were observed in all samples which can be attributed to the stress produced due to lattice distortions. The visible PL emission intensity showed appreciable enhancement with post-deposition annealing.