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1.
Jia-Hong Huang 《Surface & coatings technology》2008,202(20):4992-5000
Transition metal oxynitrides have become emerging decorative coating materials due to their adjustable coloration and high hardness and corrosion resistance. This research studied the effect of oxygen content on the coloration, mechanical properties and corrosion resistance of ZrNxOy thin films deposited on AISI 304 stainless steel using hollow cathode discharge ion plating (HCD-IP). The Zr/N/O ratios of the ZrNxOy films were determined using X-ray photoelectron spectroscopy (XPS). The color of the ZrNxOy thin film changed from golden yellow to blue and then slate blue with increasing oxygen content. X-ray diffraction (XRD) patterns revealed that phase separation of ZrN and m-ZrO2 occurred as the oxygen content reached 31.2 at.%. ZrN(O) (ZrN with dissolving oxygen) is dominant at oxygen content less than 18.1 at.%, while m-ZrO2 phase was prevailed at oxygen content above 40.3 at.%. Phase separation lowered the hardness of the ZrNxOy films as the fraction of ZrO2 was less than 40%. The residual stresses in ZrN phase was higher than that in ZrO2, and the residual stress decreased for the specimen containing 30 to 37% ZrO2. For the samples containing more than 44% ZrO2, the average residual stress was close to that in ZrO2 phase. The corrosion resistance was evaluated by salt spray test and potentiodynamic scan in two solutions: 0.5MH2SO4 + 0.05 M KSCN and 5% NaCl solutions. The results showed consistent trend in the two solutions. From the results of potentiodynamic scan, corrosion resistance increased as the packing density of the film increased, whereas the film thickness was not a crucial factor on corrosion current; moreover, the electrical conductivity of the film may be one of the significant factors in corrosion resistance. Results of salt spray tests suggested that the corrosion of ZrNxOy in NaCl may play an important role in corrosion resistance. 相似文献
2.
Nanocrystalline ZrNxOy thin films were deposited on p-type Si (100) substrates using hollow cathode discharge ion-plating (HCD-IP) and the films were annealed at 700 and 900 °C in the controlled atmosphere. The purpose of this study was to investigate the phase separation, phase transformation and the accompanying change of properties of the heat-treated ZrNxOy films deposited by ion plating. With the increase of oxygen flow rate ranging from 0 to 10 sccm, the primary phase of the as-deposited films evolved from ZrN to nearly amorphous structure and further to monoclinic ZrO2 (m-ZrO2). After heat treatment at 700 and 900 °C, phase transformation occurred in the samples deposited at 8 and 10 sccm O2, where a stoichiometric crystalline Zr2ON2 was found to derive from m-ZrO2 with dissolving nitrogen (m-ZrO2(N)). The hardness of the ZrNxOy thin films could be correlated to the fraction of Zr2ON2 + m-ZrO2. The film hardness decreased significantly as the fraction of ZrO2 + Zr2ON2 exceeded ~ 60%, which was due to phase transition by increasing oxygen flow rate or phase transformation induced by heat treatment. The phase separation of m-ZrO2 from ZrN with dissolving oxygen (ZrN(O)) may relieve the residual stress of the ZrNxOy specimens deposited at 5 and 8 sccm O2, while direct formation of m-ZrO2 increased the stress of the film deposited at 10 sccm O2. On the other hand, the phase transformation from m-ZrO2(N) to Zr2ON2 by heat treatment at both 700 and 900 °C may effectively relieve the residual stress of the ZrNxOy films. 相似文献
3.
ZrNxOy thin films were deposited on AISI 304 stainless steel (304SS) substrates by reactive magnetron sputtering. The specimens were produced by sputtering a Zr target at 500 °C and the reactive gasses were N2 and O2 at various flow rates (ranging from 0 to 2 sccm). The purpose of this study was to investigate the effect of oxygen flow rate on the phase transition and accompanying mechanical properties of the ZrNxOy thin films. The oxygen contents of the thin films increased significantly with increasing oxygen flow rate. X-ray diffraction (XRD) revealed that the characteristics of the films can be divided into three zones according to the major phase with increasing oxygen content: Zone I (ZrN), Zone II (Zr2ON2) and Zone III (m-ZrO2). The hardness of the ZrNxOy films decreased with increasing oxygen content due to the formation of the soft oxide phase. Modified XRD sin2ψ method was used to respectively measure the residual stresses of ZrN, Zr2ON2 and m-ZrO2 phases. The results showed that the residual stress in ZrN was relieved as the oxygen content increased, and Zr2ON2 and m-ZrO2 were the phases with lower residual stress. Compositional depth profiles indicated that there was a ZrO2 interlayer near the film/substrates interface for all samples except the mononitride ZrN specimen. Contact angle was used as an index to assess the wettability of the film on substrate. The contact angles of ZrN, Zr2ON2 and m-ZrO2 on stainless steel were indirectly measured using Owens-Wendt method. The results showed that ZrO2 possessed the lowest wettability on 304SS among the three ZrNxOy phases, indicating that the ZrO2 interlayer may account for the spallation of the ZrNxOy films after salt spray tests. 相似文献
4.
Ternary single-phase Bi2−xSbxSe3 alloy thin films were synthesized onto Au(1 1 1) substrates from an aqueous solution containing Bi(NO3)3, SbCl3, and SeO2 at room temperature for the first time via the electrodeposition technique. The electrodeposition of the thin films was studied using cyclic voltammetry, compositional, structural, optical measurements and surface morphology. It was found that the thin films with different stoichiometry can be obtained by controlling the electrolyte composition. The as-deposited films were crystallized in the preferential orientation along the (0 1 5) plane. The SEM investigations show that the film growth proceeds via nucleation, growth of film layer and formation of spherical particles on the film layer. The particle size and shape of Bi2−xSbxSe3 films could be changed by tuning the electrolyte composition. The optical absorption spectra suggest that the band gap of this alloy varied from 0.24 to 0.38 eV with increasing Sb content from x = 0 to x = 0.2. 相似文献
5.
L.Q. ZhangZ.Z. Ye J.Y. Huang B. LuH.P. He J.G. LuY.Z. Zhang J. JiangJ. Zhang K.W. WuW.G. Zhang 《Journal of Alloys and Compounds》2011,509(27):7405-7409
A series of K doped Zn1−xMgxO thin films have been prepared by pulsed laser deposition (PLD). Hall-effect measurements indicate that the films exhibit stable p-type behavior with duration of at least six months. The band gap of the K doped Zn1−xMgxO films undergoes a blueshift due to the Mg incorporation. However, photoluminescence (PL) results reveal that the crystallinity decreased with the increasing of Mg content. The fabricated K doped p-type Zn0.95Mg0.05O thin film exhibits good electrical properties, with resistivity of 15.21 Ω cm and hole concentration of 5.54 × 1018 cm−3. Furthermore, a simple ZnO-based p-n heterojunction was prepared by deposition of a K-doped p-type Zn0.95Mg0.05O layer on Ga-doped n-type ZnO thin film with low resistivity. The p-n diode heterostructure exhibits typical rectification behavior of p-n junctions. 相似文献
6.
The microstructure and electrical properties of BaYxBi1−xO3 thick film negative temperature coefficient thermistors, fabricated by screen printing, were investigated. The sintered thick films were the single-phase solid solutions of the BaYxBi1−xO3 compounds with a monoclinic structure. The added Y2O3 led to a significant decrease in the grain size of the thermistors. The resistivity and coefficient of temperature sensitivity for the BaYxBi1−xO3 (0 ≤ x ≤ 0.15) thick film NTC thermistors decreased first with increasing x in the range of x < 0.04 and then increased with further increase in x. 相似文献
7.
Cd1−xZnxS (0 ≤ x ≤ 1) thin films have been deposited by chemical bath deposition method on glass substrates from aqueous solution containing cadmium acetate, zinc acetate and thiourea at 80 ± 5 °C and after annealed at 350 °C. The structural, morphological, compositional and optical properties of the deposited Cd1−xZnxS thin films have been studied by X-ray diffractometer, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), photoluminescence (PL) and UV-vis spectrophotometer, respectively. X-ray diffraction analysis shows that for x < 0.8, the crystal structure of Cd1−xZnxS thin films was hexagonal structure. For x > 0.6, however, the Cd1−xZnxS films were grown with cubic structure. Annealing the samples at 350 °C in air for 45 min resulted in increase in intensity as well as a shift towards lower scattering angles. The parameters such as crystallite size, strain, dislocation density and texture coefficient are calculated from X-ray diffraction studies. SEM studies reveal the formation of Cd1−xZnxS films with uniformly distributed grains over the entire surface of the substrate. The EDX analysis shows the content of atomic percentage. Optical method was used to determine the band gap of the films. The photoluminescence spectra of films have been studied and the results are discussed. 相似文献
8.
P. ParreiraG. Lavareda A. AmaralA.M. Botelho do Rego O. CondeJ. Valente F. NunesC. Nunes de Carvalho 《Journal of Alloys and Compounds》2011,509(16):5099-5104
The effect of different mild post-annealing treatments in air, at 270 °C, for 4-6 min, on the optical, electrical, structural and chemical properties of copper sulphide (CuxS) thin films deposited at room temperature are investigated. CuxS films, 70 nm thick, are deposited on glass substrates by vacuum thermal evaporation from a Cu2S:S (50:50 wt.%) sulphur rich powder mixture. The as-deposited highly conductive crystalline CuS (covellite) films show high carrier concentration (∼1022 cm−3), low electrical resistivity (∼10−4 Ω cm) and inconclusive p-type conduction. After the mild post-annealing, these films display increasing values of resistivity (∼10−3 to ∼10−2 Ω cm) with annealing time and exhibit conclusive p-type conduction. An increase of copper content in CuxS phases towards the semiconductive Cu2S (chalcocite) compound with annealing time is reported, due to re-evaporation of sulphur from the films. However, the latter stoichiometry was not obtained, which indicates the presence of vacancies in the Cu lattice. In the most resistive films a Cu2O phase is also observed, diminishing the amount of available copper to combine with sulphur, and therefore the highest values of optical transmittance are reached (65%). The appearance on the surface of amorphous sulphates with annealing time increase is also detected as a consequence of sulphur oxidation and replacement of sulphur with oxygen. All annealed films are copper deficient in regards to the stoichiometric Cu2S and exhibit stable p-type conductivity. 相似文献
9.
Ching-Fang Tseng 《Journal of Alloys and Compounds》2011,509(39):9447-9450
The influence of Zr substitution for Ti on the microwave dielectric properties and microstructures of the Mg(ZrxTi1−x)O3(MZxT) (0.01 ≤ x ≤ 0.3) ceramics was investigated. The quality factors of Mg(ZrxTi1−x)O3 ceramics with x = 0.01-0.05 were improved because the solid solution of a small amount of Zr4+ substitution in the B-site could increase density and grain size. An excess of Zr4+ resulted in the formation of a great deal of secondary phase that declined the microwave dielectric properties of MZxT ceramics. The temperature coefficient of resonant frequency (τf) of Mg(ZrxTi1−x)O3 ceramics slightly increased with increasing Zr content, and the variation in τf was attributed to the formation of secondary phases. 相似文献
10.
The formation of impurity LixNi1−xO when synthesizing spinel LiNi0.5Mn1.5O4 using solid state reaction method, and its influence on the electrochemical properties of product LiNi0.5Mn1.5O4 were studied. The secondary phase LixNi1−xO emerges at high temperature due to oxygen deficiency for LiNi0.5Mn1.5O4 and partial reduction of Mn4+ to Mn3+ in LiNi0.5Mn1.5O4. Annealing process can diminish oxygen deficiency and inhibit impurity LixNi1−xO. The impurity reduces the specific capacity of product, but it does not have obvious negative effect on cycle performance of product. The capacity of LiNi0.5Mn1.5O4 that contains LixNi1−xO can deliver about 120 mAh g−1. 相似文献
11.
Ag-doped Ca3Co4O9 thin films with nominal composition of Ca3−xAgxCo4O9 (x = 0∼0.4) have been prepared on sapphire (0 0 0 1) substrates by pulsed laser deposition (PLD). Structural characterizations and surface chemical states analysis have shown that Ag substitution for Ca in the thin films can be achieved with doping amount of x ≤ 0.15; while x > 0.15, excessive Ag was found as isolated and metallic species, resulting in composite structure. Based on the perfect c-axis orientation of the thin films, Ag-doping has been found to facilitate a remarkable decrease in the in-plane electrical resistivity. However, if doped beyond the substitution limit, excessive Ag was observed to severely reduce the Seebeck coefficient. Through carrier concentration adjustment by Ag-substitution, power factor of the Ag-Ca3Co4O9 thin films could reach 0.73 mW m−1 K−2 at around 700 K, which was about 16% higher than that of the pure Ca3Co4O9 thin film. 相似文献
12.
CuCr1−xMgxO2 (x = 0, 0.03, 0.05, 0.07) thin films were prepared on sapphire substrates by sol-gel processing. The effect of Mg concentrations on the structural, morphological, electrical and optical properties was investigated. Highly transparent ≧70% Mg-doped CuCrO2 thin films with p-type conduction and semiconductor behavior were obtained. The microstructure of the systems was characterized by scanning electron microscopy and the roughness increased as the content of Mg increased. The photoluminescence spectra results indicated that it had a green luminescent emission peak at the 530 nm. In this paper, CuCr0.95Mg0.05O2 film has the lowest resistivity of 7.34 Ω cm with direct band gap of 3.11 eV. In order to investigate the conduction mechanism, the energy band of the CuCrO2 films is constructed based on the grain-boundary scattering. 相似文献
13.
Nanostructured TiN/CNx multilayer films were deposited onto Si (100) wafers and M42 high-speed-steel substrates using closed-filed unbalanced magnetron sputtering in which the deposition process was controlled by a closed loop optical emission monitor (OEM) to regulate the flow of N2 gas. Multilayers with different carbon nitride (CNx) layer thickness could be attained by varying the C target current (0.5 A to 2.0 A) during the deposition. It was found that the different bilayer thickness periods (i.e. the TiN layer thickness ΛTiN was fixed at 3.0 nm while the CNx layer thickness ΛCNx was varied from 0.3 to 1.2 nm) significantly affected the mechanical and tribological properties of TiN/CNx multilayer films. These multilayer films were characterized and analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), atomic force microscopy (AFM), Rockwell-C adhesion test, scratch test, pin-on-disc tribometer, and nanoindentation measurements. XPS analyses revealed that the chemical states, such as TiN, TiC, TiNxOy and TiO2, existed in a TiN layer. Nanoindentation results showed that the hardness was highly dependent on the bilayer thickness. A maximum hardness of ~ 41.0 GPa was observed in a multilayer film at bilayer thickness ΛTiN = 3.0 nm and ΛCNx = 0.9 nm. All multilayer films exhibited extreme elasticity with elastic recoveries as high as 80% at 5 mN maximum load. The compressive stresses in the films (in a range of 1.5-3.0 GPa) were strongly related to their microstructure, which depended mainly on the incorporation of nitrogen in the films. By scratch and Rockwell-C adhesion tests, the multilayer films with smaller bilayer thicknesses (ΛTiN = 3.0 nm, ΛCNx = 0.3 and 0.6 nm) exhibited the best adhesion and cohesive strength. The critical load value obtained was as high as ~ 78 N for the films with ΛTiN = 3.0 nm, ΛCNx = 0.9 nm. The friction coefficient value for a multilayer at ΛTiN = 3.0 nm and ΛCNx = 0.9 nm was found to be low 0.11. These adhesive properties and wear performance are also discussed on the basis of microstructure, mechanical properties and tribochemical wear mechanisms. 相似文献
14.
In this paper, the chosen composition of PZT film falls in rhombohedral phase region and the dependence of lattice distortion on film thickness in sol-gel derived Pb(Zr0.58Ti0.42)O3 thin films was systematically investigated. The results confirm that the Pb(Zr0.58Ti0.42)O3 films have monoclinic phase even though the composition falls in the rhombohedral phase region. The mixed textures of (1 0 0) and (1 1 1) occur in the PZT films. In the case of mixed textures, a method using ψ-scan XRD to characterize the phase type of Pb(Zr0.58Ti0.42)O3 film is presented. It is found that the phase type of (1 0 0)-oriented grains is MA phase, and that of (1 1 1)-oriented grains is MB phase. Moreover, the lattice constants of both MA and MB phases are sensitive to the film thickness. The lattice distortion of monoclinic phase becomes smaller as film thickness increases. 相似文献
15.
Hengzhi ChenBin Yang Mingfu ZhangFeiyan Wang Kokwai CheahWenwu Cao 《Journal of Alloys and Compounds》2011,509(17):5364-5367
Lanthanum doped Bi3TiNbO9 thin films (LBTN-x, La3+ contents x = 5%, 15%, 25% and 35 mol.%) with layered perovskite structure were fabricated on fused silica by pulsed laser deposition method. Their linear and nonlinear optical properties were studied by transmittance measurement and Z-Scan method. All films exhibit good transmittance (>55%) in visible region. For lanthanum doping content are x = 5%, 15% and 25 mol.%, the nonlinear absorption coefficient of LBTN-x thin films increases with the La3+ content, then it drops down at x = 35 mol.% when the content of La3+ in (Bi2O2)2+ layers is high enough to aggravate the orthorhombic distortion of the octahedra. We found that, 25 mol.% is the optimal La3+ content for LBTN-x thin films to have the largest nonlinear absorption coefficient making the LBTN-x film a promising candidate for absorbing-type optical device applications. 相似文献
16.
Pb(ZrxTi1−x)O3 thin films with mixed orientations of (1 1 1) and (1 0 0) were prepared on Pt/Ti/SiO2/Si substrate by sol-gel technique. The compositions of PZT thin films are chosen as x = 0.55 and x = 0.58. Both of the compositions are in the rhombohedral phase region of the Pb(ZrxTi1−x)O3 phase diagram, but the former is near the monoclinic phase existence region, and the latter is far from the monoclinic phase existence region. Rhombohedral-monoclinic phase transitions are reported in both of the thin films. The results show that the phase transition is related to the grain orientation. Phase transitions in the films are clearly identified: rhombohedral phase transforms to MB phase in (1 1 1)-oriented grains, and rhombohedral phase transforms to MA phase in (1 0 0)-oriented grains. The remnant polarization is determined by the content of (1 1 1)-oriented grains. It is shown that the remnant polarization is greater in the film with higher content of (1 1 1)-oriented grains. 相似文献
17.
(ZrO2)1−x(Y2O3)x thin films were sputter-deposited from metallic targets in various reactive argon-oxygen gas mixtures. Structural investigations have been realised by X-ray Diffraction (XRD), Raman spectroscopy and Transmission Electron Microscopy (TEM). The coatings microstructure have been characterised by TEM and their morphology by Scanning Electron Microscopy (SEM) on brittle-fracture cross sections. Chemical compositions have been achieved by Electron Probe Micro-Analysis (EPMA) and by Energy Dispersive Spectroscopy (EDS). Finally, attention was paid to the film optical properties, as assessed via Optical Transmission Interferometry (OTI) as well as spectrophotometry.In a first part, we have studied the influence of the argon pressure on the chemical, structural and morphological properties of the coatings. In a second part, we have observed the effect of the yttria content on the structure of the films. 相似文献
18.
J. Olejní?ek L.E. FlanneryS.A. Darveau C.L. ExstromŠ. Kment N.J. IannoR.J. Soukup 《Journal of Alloys and Compounds》2011,509(41):10020-10024
CuIn1−xAlxS2 thin films (x = 0, 0.09, 0.27, 0.46, 0.64, 0.82 and 1) with thicknesses of approximately 1 μm were formed by the sulfurization of DC sputtered Cu-In-Al precursors. All samples were sulfurized in a graphite container for 90 min at 650 °C in a 150 kPa Ar + S atmosphere. Final films were studied via X-ray diffraction (XRD), scanning electron microscopy (SEM) and micro-Raman spectroscopy. It was found that all samples were polycrystalline in nature and their lattice parameters varied slightly nonlinearly from {a = 5.49 Å, c = 11.02 Å} for CuInS2 to {a = 5.30 Å, c = 10.36 Å} for CuAlS2. No unwanted phases such as Cu2−xS or others were observed. Raman were recorded at a room temperature and the most intensive and dominant A1 phonon frequency varied nonlinearly from 294 cm−1 (CuInS2) to 314 cm−1 (CuAlS2). 相似文献
19.
Preparation of the Ti3Si1−xAlxC2 solid solution with x = 0.2-0.8 was investigated by self-propagating high-temperature synthesis (SHS) using TiC-, SiC-, and Al4C3-containing powder compacts. Due to the variation of reaction exothermicity with sample stoichiometry, the combustion temperature and reaction front velocity decreased with increasing Al content of Ti3Si1−xAlxC2 for the TiC- and Al4C3-added samples, but increased for the samples with SiC. In contrast to the formation of Ti3(Si,Al)C2 as the dominant phase for the TiC- and SiC-added samples, TiC was identified as the major constituent in the final products of samples adopting Al4C3. In addition, the evolution of Ti3(Si,Al)C2 was improved by increasing the Al content of the TiC- and SiC-added powder compacts, but deteriorated considerably upon the increase of Al4C3 in the Al4C3-containing sample. 相似文献
20.
Wenting Liu Zhengtang Liu Feng Yan Tingting Tan Hao Tian 《Surface & coatings technology》2010,205(7):2120-2125
Hafnium dioxide (HfO2) thin films were deposited on a quartz substrate by RF reactive magnetron sputtering. The influence of O2/Ar flow ratio on the deposition rate, structure and optical properties of HfO2 thin films were systematically studied using X-ray diffraction (XRD), scan electron microscopy (SEM) and UV-visible spectroscopy. The results show that the deposition rate decreases obviously when the O2/Ar flow ratio increases from 0 to 0.25 and then, decreases little as the O2/Ar flow ratio further increases to 0.50. The HfO2 thin films prepared are all polycrystalline with a monoclinic phase. The thin film deposited with pure argon shows a preferential growth and has considerably improved crystallinity and much larger crystallite size. Meanwhile, after oxygen is introduced into the deposition, the thin films prepared have random orientation, weakened crystallinity and smaller crystallite size. The refractive index is higher for the thin film deposited without oxygen and increases as the O2/Ar flow ratio increases from 0.25 to 0.50. The band gap energy of the thin film increases with an increasing O2/Ar flow ratio. 相似文献