Influence of Annealing Temperature on the Microstructure and Morphology of TiN Films Synthesized by Dual Magnetron Sputtering

TiN films synthesized on leucosapphire substrates by dual magnetron sputtering have been annealed in vacuum at 600, 700, 800, and 900°C for 2 min. The microstructure and morphology of the films have been studied by X-ray diffraction and scanning electron microscopy at different temperatures. It has been found that annealing changes the microstructure, texture, grain size, and surface roughness of the TiN films.     

GaAs/SiO_2超晶格的制备和Raman光谱研究

我们采用射频磁控溅射方法在 p- Si衬底上成功地制备出四周期的非晶 Ga As/Si O2超晶格 ,并取得其高分辨率电镜像。以 80 0℃快速退火方法使超晶格中非晶的 Ga As层局部晶化 ,利用 Raman散射谱研究了其结构变化。     

Annealing induced transformations in structural and optical properties of Ge30Se70−xBix thin films

ABSTRACT

Thin films of Ge₃₀Se_70?xBi_x (x?=?5, 15, 20) were prepared by thermal evaporation method on glass substrates with thickness 800?nm. The films were annealed at 250°C and 320°C for 2?h to study the annealing-induced structural and optical change. The X-ray diffraction characterization revealed the amorphous to crystalline phase transformation with annealing. The indirect optical band gap decreased with annealing which is explained on the basis of phase transformation and density of localized states. The formation of surface dangling bonds around the crystallites during crystallization process reduced the band gap. The Tauc parameter and Urbach energy change show the degree of chemical disorderness in the films. The transmitivity decreased while the absorption coefficient increased with the annealing process. The microstructural study done by Field emission scanning electron microscopy shows the formation of crystallites upon annealing. Atomic force microscopy investigation on these films shows the influence of annealing on surface topography.     

Changes of structure and composition of a zinc ion-implanted silicon surface during nanoparticle formation upon thermal treatment

Data from investigating the formation of nanoparticles (NPs) on a surface of silicon wafers after zinc ion implantation and thermal annealing are presented. The investigation is conducted by means of trans-mission electron microscopy, electron diffraction analysis, energy dispersive microanalysis, scanning tunneling microscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. It is found that on their surfaces, the implanted samples have only films of amorphous silicon containing implanted zinc, oxygen, and carbon contamination. Thermal treatment in the range of 400–800°C leads to the formation NP with 20–50 nm wide and 10 nm tall on a wafer’s surface, plus a silicon oxide layer about 20 nm thick. NPs are composed of zinc compounds of the ZnO, ZnSiO₃, or Zn₂SiO₄ types. These NPs disappear after annealing at 1000°C.     

Effect of N2 ambient annealing on the field emission properties of HfNxOy thin films

HfN_xO_y thin films were deposited on Si substrates by direct-current sputtering. The influence of N₂ ambient annealing on the morphology, structure and field emission properties of the HfN_xO_y thin films was studied systematically. Scanning electron microscopy indicates that both the as-deposited and the annealed films are composed of nanoparticles, and the particle sizes of these films do not change much before and after annealing. Atomic force microscopy shows that the surface of the as-deposited films is smooth while that of the annealed films becomes rough, with many protrusions. X-ray diffraction patterns demonstrate that the as-deposited films are amorphous while the samples annealed at over 500 °C are polycrystalline. It is found that the field electron emission properties of the annealed films are better than those of the as-deposited films. The film annealed at 800 °C shows the best field emission properties. The mechanism for the improvement of the field electron emission property of the annealed thin films is also discussed. PACS 73.61.-r; 79.70.+q; 81.05.-t     

Surface morphology of ZnO buffer layer and its effects on the growth of GaN films on Si substrates by magnetron sputtering

ZnO thin films were first prepared on Si(111) substrates using a radio frequency magnetron sputtering system. Then the as-grown ZnO films were annealed in oxygen ambient at temperatures of 700, 800, 900, and 1000°C , respectively. The morphologies of ZnO films were studied by an atom force microscope (AFM). Subsequently, GaN epilayers about 500 nm thick were deposited on the ZnO buffer layers. The GaN/ZnO films were annealed in NH₃ ambient at 900°C. The microstructure, morphology and optical properties of GaN films were studied by x-ray diffraction (XRD), AFM, scanning electron microscopy (SEM) and photoluminescence (PL). The results are shown, their properties having been investigated particularly as a function of the ZnO layers. For better growth of the GaN films, the optimal annealing temperature of the ZnO buffer layers was 900°C.     

Physical properties of vacuum evaporated CdTe thin films with post-deposition thermal annealing

This paper presents the physical properties of vacuum evaporated CdTe thin films with post-deposition thermal annealing. The thin films of thickness 500 nm were grown on glass and indium tin oxide (ITO) coated glass substrates employing thermal vacuum evaporation technique followed by post-deposition thermal annealing at temperature 450 °C. These films were subjected to the X-ray diffraction (XRD),UV-Vis spectrophotometer, source meter and atomic force microscopy (AFM) for structural, optical, electrical and surface morphological analysis respectively. The X-ray diffraction patterns reveal that the films have zinc-blende structure of single cubic phase with preferred orientation (111) and polycrystalline in nature. The crystallographic and optical parameters are calculated and discussed in brief. The optical band gap is found to be 1.62 eV and 1.52 eV for as-grown and annealed films respectively. The I–V characteristics show that the conductivity is decreased for annealed thin films. The AFM studies reveal that the surface roughness is observed to be increased for thermally annealed films.     

Effect of annealing time on properties of spinel LiNi<Subscript>0.5</Subscript>Mn<Subscript>1.5</Subscript>O<Subscript>4</Subscript> high-voltage lithium-ion battery electrode materials prepared by co-precipitation method

In this wok, a series of LiNi_0.5Mn_1.5O₄ (LNMO) samples with an octahedral shape entirely composed of (111) crystal planes were prepared by calcining the mixture of the precursor Ni_0.25Mn_0.75(OH)₂ and LiOH·H₂O at 800 °C for 15 h in air, followed by annealing them at 600 °C for different dwelling times. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and several electrochemical technologies were used to investigate the effect of annealing time on properties of the LNMO samples. XRD analysis indicates that the lattice parameters of the LNMO samples show a decreasing trend with increasing of annealing time, and the impurity peaks become less apparent for the sample annealed for 6 h and almost disappear for the samples annealed for 9 and 24 h. SEM results show that the annealing time has no obvious influence on the morphologies of the LNMO samples. Electrochemical measurements show that the electrochemical performances (capacity, cycle life, and rate capability) of the samples annealed for 6, 9, and 24 h are better than those of the unannealed sample, and the sample annealed for 9 h shows the best electrochemical properties among them due to its superior electrochemical kinetics of Li⁺ insertion/desertion.     

Ultrathin amorphous Ti–Al film used as a diffusion barrier for copper metallization

The viability of ultrathin amorphous Ti–Al film (～4 nm) as a diffusion barrier layer between Cu and Si for the application in Si-based ultra-large scale integration (ULSI) has been investigated. The Cu/Ti–Al/Si heterostructures are annealed in a high vacuum at various temperatures. There is no impurity peaks in the X-ray diffraction patterns for the samples up to annealing temperature of 800 ^°C, although the island-like grains were observed on the surface of the 800 ^°C annealed sample due to dewetting and agglomeration of the Cu film. No inter-reactions can be found from the images of transmission electron microscopy and Ti–Al is still amorphous after high-temperature annealing. These results indicate that Ti–Al film can effectively separate Cu from Si at high temperatures, and that the amorphous ultrathin Ti–Al film can be a very good barrier layer for Cu metallization.     

Optical constants of vacuum annealed radio frequency (RF) magnetron sputtered zinc oxide thin films

Zinc oxide thin films were deposited by radio frequency magnetron sputtering. The films were annealed in vacuum at temperatures of 400, 600, and 800 °C. The influence of annealing on the structural, chemical, and optical properties of the films was investigated. From a structural point of view, the films were highly oriented, with columnar microstructure. Chemical analysis indicated that the films were sub-stoichiometric, and that the concentration of oxygen vacancies was enhanced upon annealing. The films were highly transparent in the visible and near-infrared spectral regions. Transparency was reduced as the annealing temperature was increased. The refractive index and extinction coefficient, in the transparent regions of the films, were derived from transmittance measurements. The refractive index manifested variation that was affected by crystallite size, roughness and defect concentration. The extinction coefficient of the as-deposited films and those annealed at 400 °C was negligible. However, the films annealed at 600 or 800 °C had much larger values of the extinction coefficient due to increased absorption or scattering. The absorption coefficient and optical band gap of the films were derived from spectrophotometric measurements. The absorption coefficient showed progressive increase with the annealing temperature. However, the band gap did not show significant variation.     

Pulsed laser deposition of molybdenum oxide thin films

Thin films of molybdenum oxide were deposited in vacuum by pulsed laser ablation using a xenon fluoride (351 nm) and a krypton fluoride (248 nm) excimer lasers. The films were deposited on unheated substrates and were post-annealed in air in the temperature range 300–500°C. The structural, morphological, chemical, and optical properties of the films were studied. As-deposited films were found to be dark. The transparency of the films was improved with annealing in air. The films were polycrystalline with diffraction peaks that belong to the orthorhombic phase of MoO₃. The surface morphology of the films showed a layered structure. Both the grain size and surface roughness increased with annealing temperature. The stoichiometry of the films improved upon annealing in air, with the best stoichiometry of MoO_2.95 obtained for films deposited by the XeF laser and annealed at 400°C. Similarly, the best transparency, with a transmittance exceeding 80%, was obtained with the films annealed in the temperature range 400–450°C.     

Effect of annealing on photo accelerated chemically deposited Indium sulfide thin films with various cationic precursors

The present work reports the deposition of Indium sulfide thin films by a recently established novel method called photo-assisted chemical deposition technique. It is a very low cost method for the deposition of thin films, and can be easily scaled up for industrial production. Indium sulfide thin films are deposited on glass substrates through various cationic precursors and the effect of annealing on structural, optical and morphological properties was investigated. Films have been characterized with respect to their structural, optical and morphological properties by means of X-ray diffraction, UV–VIS-NIR Spectrophotometer, SEM and AFM techniques. As-deposited films on glass substrates were amorphous and became crystalline after annealing. The grain size of all the annealed films are larger than the as-prepared films and attained a maximum value for the film prepared with sulfate precursor. The calculated strain was compressive in nature. Surface roughness was estimated from the AFM measurements and found to be decreased in annealed samples. The film deposited with chloride precursor showed a higher visible transmittance of around 80 % and became 90 % on annealing. The variation of packing density follows the variation of the refractive index. The optical band gap of the samples was estimated and found to be within the range of 2.45–2.71 eV, which is in quite agreement with the literature.     

Microstructural and surface property variations due to the amorphous region formed by thermal annealing in Al-doped ZnO thin films grown on n-Si (1 0 0) substrates

X-ray diffraction (XRD) patterns revealed that the as-grown and annealed Al-doped ZnO (AZO) films grown on the n-Si (1 0 0) substrates were polycrystalline. Transmission electron microscopy (TEM) images showed that bright-contrast regions existed in the grain boundary, and high-resolution TEM (HRTEM) images showed that the bright-contrast regions with an amorphous phase were embedded in the ZnO grains. While the surface roughness of the AZO film annealed at 800 °C became smoother, those of the AZO films annealed at 900 and 1000 °C became rougher. XRD patterns, TEM images, selected-area electron diffraction patterns, HRTEM images, and atomic force microscopy (AFM) images showed that the crystallinity in the AZO thin films grown on the n-Si (1 0 0) substrates was enhanced resulting from the release in the strain energy for the AZO thin films due to thermal annealing at 800 °C. XRD patterns and AFM images show that the crystallinity of the AZO thin films annealed at 1000 °C deteriorated due to the formation of the amorphous phase in the ZnO thin films.     

Effect of sputtering pressure on structural and optical properties of silver oxide thin films; Kramers–Kronig method

Silver oxide nano layers were prepared by RF magnetron sputtering on amorphous SiO₂ substrates. O₂ pressure in chamber was varied from 1 to 4 and 7 mTorr during growth process. The effects of different O₂ pressure on structural, morphological and optical properties of the films were investigated by means of X-ray diffraction, scanning electron microscopy, atomic force microscopy and UV–Vis spectroscopy analyses. Optical reflectance measured in the wavelength of 350–950 nm by spectroscopy. Other optical properties and optical band gaps were calculated using Kramers–Kronig relations. The X-ray diffraction measurements showed change in crystalline structure with increasing O₂ pressure. Preferred orientation has been changed to another growth orientation at 4 mTorr O₂ pressure. The Atomic force microscope images showed increasing in roughness consistently by increasing oxygen pressure. The thickness of the thin films decreases (from 217 to 180 nm) with increasing O₂ pressure. Optical results revealed that the highest optical band gap of 3.1 eV and the highest transmittance of?~?80% were achieved at lower O₂ pressure (1 mTorr).     

Thermal stability of second generation carbosilane dendrimers with peripheral ammonia groups

Spinel nickel zinc ferrite nanowires were successfully prepared in mesoporous silica SBA-15 as a host matrix. The powder was annealed at a range of temperatures (500–900 °C) with heating rate 0.5 °C/min. The required NiZnFe₂O₄ phase was obtained at 700 °C. The specific surface area S_BET data revealed that the surface area of the mesoporous silica after annealing was decreased from 821 to 90 m²/g which indicated that the spinal ferrite fills the channels of mesoporous materials. The one-dimensional spinel nanostructures were characterized by X-ray diffraction, infrared spectroscopy, vibrating sample magnetometer, and transmission electron microscopy before and after a selective removal of the silica template in aqueous solution of NaOH or HF. The presence of SBA-15 lowers the formation temperature of nickel zinc ferrite nanowires compared to the corresponding bulk material. The magnetic properties revealed a high saturation magnetization level (~43 emu/g) for the Ni–Zn nanowires at 900 °C.     

Fractal analysis and atomic force microscopy measurements of surface roughness for Hastelloy C276 substrates and amorphous alumina buffer layers in coated conductors

In coated conductors, surface roughness of metallic substrates and buffer layers could significantly affect the texture of subsequently deposited buffer layers and the critical current density of superconductor layer. Atomic force microscopy (AFM) is usually utilized to measure surface roughness. However, the roughness values are actually relevant to scan scale. Fractal geometry could be exerted to analyze the scaling performance of surface roughness. In this study, four samples were prepared, which were electro polished Hastelloy C276 substrate, mechanically polished Hastelloy C276 substrate and the amorphous alumina buffer layers deposited on both the substrates by ion beam deposition. The surface roughness, described by root mean squared (RMS) and arithmetic average (R_a) values, was analyzed considering the scan scale of AFM measurements. The surfaces of amorphous alumina layers were found to be fractal in nature because of the scaling performance of roughness, while the surfaces of Hastelloy substrates were not. The flatten modification of AFM images was discussed. And the calculation of surface roughness in smaller parts divided from the whole AFM images was studied, compared with the results of actual AFM measurements of the same scan scales.     

Influence of surface topography and annealing temperature on the surface and volume of dissipation electrical energy and Spitzer–Fan model in Al doped ZnO films

The aim of this work is to investigate the optical constants of aluminum doped zinc oxide films annealed at different temperatures. With increasing temperature, due to decreasing unfilled inter-granular volume per unit thickness, the optical transmittance spectra of films were increased. The films have a normal dispersion in the spectral range 400?<?λ?<?500 nm and the anomalous dispersion in IR range. The lattice dielectric constants ε_L, the free charge carriers concentration, the plasma frequency, Spitzer–Fan model and the waste of electrical energy as heat of films can be analyzed using the refractive index n and the extinction coefficient k spectra. With increasing annealing temperature, the lattice dielectric constants ε_L of films decrease however the free charge carriers concentration of films increase. The free carrier electric susceptibility of films annealed at 600 °C has maximum value. The energy loss by the free charge carriers when traversing the bulk and surface of films annealed at 600 °C has a minimum value in the near fundamental absorption edge and it with increasing energy increases.     

Influence of Annealing Treatment on Structural,Optical, Electric,and Thermoelectric Properties of MBE-Grown ZnO

In this paper, we have reported the influence of annealing treatment on structural, optical, electrical, and thermoelectric properties of MBE-grown ZnO on Si substrate. After growth, a set of as grown ZnO was annealed in oxygen environment at 500–800°C and another set was annealed in different environments (vacuum, oxygen, zinc, and vacuum + zinc) at 600°C for one hour in a programmable furnace. X-ray diffraction (XRD) results demonstrated that all annealed samples exhibited a major diffraction peak related to (002) plane. The full width at half maximum (FWHM) of this plane decreased and crystalline size increased for oxygen annealed sample and it increased when samples were annealed in zinc, vacuum, and successively annealed in vacuum and zinc. Further, photoluminescence spectrum revealed that the intensity of band edge emission increased and defect emission decreased as annealing temperature (oxygen environment) increased while it decreased for rest of annealing ambient. It is suspected that annealing in oxygen environment causes compensation of the oxygen vacancies by the incoming oxygen flux, while annealing in zinc and vacuum generates more oxygen vacancies. Hall and Seebeck measurements are also consistent with these arguments.     

Growth and Characterization of High-Quality Dielectric Sputtered Zinc Oxide Films from the First Principle

In this article, we investigate the effect of thermal treatment on a piezoelectric material, zinc oxide, which has found numerous applications in sensors and actuators. Even though the exact mechanisms rendering electrical properties are less known, we suspect that the thermal treatments are responsible for improvement of electrical characteristics of the deposited thin films. We establish that the thermal agitation is responsible for improvement of orders of magnitude in electrical characteristics of sputtered ZnO thin films. The surface quality of the thin films deposited is process dependent. ZnO films were deposited using a dielectric sputtering method, on oxidized silicon 100 n-type wafers. Further, these films were thermally annealed in oxygen ambient at 600 °C in a tube furnace with 2 mL/min pressure. It is observed that, after thermal annealing, the quality of the films is improved by orders of magnitude. The luminance, crystalline quality, and surface morphology of these thin films was measured with atomic force microscopy, scanning electron microscopy with BSD detector (BSD-SEM), and Fourier transform infrared spectroscopy (FTIR). The results infer that the film’s surface is very smooth and dense. The surface roughness is improved by 1.3149 nm from 7.882 nm prior to thermal annealing to post-annealing surface roughness with 6.5671 nm. Post-thermal annealing process reveals average grain size was 50 nanometers; the surface roughness is reduced to 6.5671 nm. A significant improvement in electrical current-voltage characteristics was recorded with I-V curve. It is suspected to be due to substantial enhancement in electrical conductivity as a result of thermal treatment and improved spectral response recorded a FTIR peak shift of 1 wave number in total. The FTIR peak shift is suspected to be due to evaporation and reduction in oxygen vacancies due to thermal annealing process. The post-annealed ZnO films will be used for actuation in the future.     

Effect of annealing on electrical resistivity of rf-magnetron sputtered nanostructured SnO2 thin films

Tin oxide (SnO₂) thin films were deposited by radio frequency (RF) magnetron sputtering on clean corning glass substrates. These films were then annealed for 15 min at various temperatures in the range of 100-500°C. The films were investigated by studying their structural and electrical properties. X-ray diffraction (XRD) results suggested that the deposited SnO₂ films were formed by nanoparticles with average particle size in the range of 23-28 nm. XRD patterns of annealed films showed the formation of small amount of SnO phase in the matrix of SnO₂. The initial surface RMS roughness measured with atomic force microscopy (AFM) was 25.76 nm which reduces to 17.72 nm with annealing. Electrical resistivity was measured as a function of annealing temperature and found to lie between 1.25 and 1.38 mΩ cm. RMS roughness and resistivity show almost opposite trend with annealing.