Structural and optical analysis of ZnBeMgO powder and thin films

We here report the structural and optical studies of Zn_1−x−yBe_xMg_yO (0 ≤ x ≤ 0.15; 0 ≤ y ≤ 0.20) powders and thin films. From the Rietveld refinement of the powder X-ray diffraction (XRD) patterns it was revealed that the value of ‘a’ lattice parameter remains almost unchanged whereas ‘c’ parameter reduces with Be and Mg co-doping in ZnO. The Zn-O bond length also decreases in co-doped samples. Raman studies of the pure ZnO powder showed all the characteristic peaks of the wurtzite hexagonal structure and with (Be, Mg) co-doping new modes appeared which can be attributed to arise as a result of substitution. The XRD of the films prepared from the powders using pulsed laser deposition (PLD) technique exhibited the preferential orientation and with increase in co-doping the (0 0 0 2) peak also shifts to higher 2θ values suggesting the incorporation of Be/Mg at the Zn-site. From the UV-visible optical transmittance measurement it was noticed that the band gap of the pristine ZnO film is 3.3 eV which enhanced up to 4.51 eV for Zn_0.7Be_0.1Mg_0.2O film which lies in the solar blind region and is very useful in the realization of deep UV detectors.     

Structural, optical and electrical properties of N-doped ZnO thin films prepared by thermal oxidation of pulsed filtered cathodic vacuum arc deposited ZnxNy films

In this study, N-doped ZnO thin films were fabricated by oxidation of Zn_xN_y films. The Zn_xN_y thin films were deposited on glass substrates by pulsed filtered cathodic vacuum arc deposition (PFCVAD) using metallic zinc wire (99.999%) as a cathode target in pure nitrogen plasma. The influence of oxidation temperature, on the electrical, structural and optical properties of N-doped ZnO films was investigated. P-type conduction was achieved for the N-doped ZnO obtained at 450 °C by oxidation of Zn_xN_y, with a resistivity of 16.1 Ω cm, hole concentration of 2.03 × 10¹⁶ cm⁻³ and Hall mobility of 19 cm²/V s. X-ray photoelectron spectroscopy (XPS) analysis confirmed the incorporation of N into the ZnO films. X-ray diffraction (XRD) pattern showed that the films as-deposited and oxidized at 350 °C were amorphous. However, the oxidized films in air atmosphere at 450-550 °C were polycrystalline without preferential orientation. In room temperature photoluminescence (PL) spectra, an ultraviolet (UV) peak was seen for all the samples. In addition, a broad deep level emission was observed.     

The effect of NH3 concentrations on the electrical properties of N-doped ZnO and study on mechanism

The N-doped ZnO films deposited by RF magnetron sputtering were treated under various NH₃ concentrations. The N-doped ZnO films were characterized by XRD, FESEM, Hall measurement and XPS. The XRD and SEM results showed that ZnO films were crystallized in the wurzite phase with a preferential orientation along the c axis and the surfaces were smooth and dense over the film. The Hall and XPS measurement indicated that N element had doped into ZnO crystal lattice, which is benefit for fabrication of p type ZnO films.     

Morphology and optical properties of Co doped ZnO textured thin films

Depending on the ZnO seed-layers, a new kind of cobalt doped zinc oxide (Zn_1−xCo_xO) thin films with controllable morphology were prepared by a facile solvothermal method. A series of ZnO thin films with different Co contents were applied to study the effect of doped Co on morphology, structural and optical properties. It is found that the doped content plays an important role on morphology evolution of Zn_1−xCo_xO films. The results of scanning electron microscope (SEM) indicate that the Zn_1−xCo_xO films are highly uniform and porous. Co has been successfully doped into the ZnO lattice structure and revealed by X-ray diffraction (XRD) and energy dispersive spectrum (EDS). It can be found that Zn_1−xCo_xO thin films possess good crystalline quality through the characterization of transmission electron microscope (TEM) and high-resolution transmission electron microscopy (HRTEM). All of the samples show a stronger violet emission and ultraviolet absorption, and the violet emission peaks shift towards red with increasing of Co content. In addition, the magnetic result demonstrates that the prepared Co-doped ZnO thin films are room-temperature ferromagnetic materials.     

Annealing temperature dependence of the optical and structural properties of selenium-rich CdSe thin films

Structural and optical properties of selenium-rich CdSe (SR-CdSe) thin films prepared by thermal evaporation are studied as a function of annealing temperature. X-ray diffraction (XRD) patterns show that the as-prepared films were amorphous, whereas the annealed films are polycrystalline. Analyzing XRD patterns of the annealed films reveal the coexistence of both (hexagonal) Se and (hexagonal) CdSe crystalline phases. Surface roughness of SR-CdSe films is measured using atomic force microscope (AFM). Analyses of the absorption spectra in the wavelength range (200-2500 nm) of SR-CdSe thin films indicates the existence of direct and indirect optical transition mechanisms. The optical band gap (E_g) of as-prepared film is 1.92 and 2.14 eV for the indirect allowed and direct allowed transitions respectively. After annealing, the absorption coefficient and optical band gap were found to decrease, while the values of refractive index (n) and the extinction coefficient (k_ex) increase. The dispersion of the refractive index is described using the Wimple-Di Domenico (WDD) single oscillator model and the dispersion parameters are calculated as a function of annealing temperature. Besides, the high frequency dielectric constant (?_∞) and the ratios of the free carrier concentration to its effective mass (N/m*) are studied as a function of annealing temperature. The results are discussed and correlated in terms of amorphous-crystalline transformations.     

Electrodeposition of black chromium from environmentally electrolyte based on trivalent chromium salt

Thin films of black chromium have been prepared by electrodeposition technique on steel substrates. Deposition of 1 µm thickness is conducted in a solution of chromium trivalent salt and oxidizing agent fluorosilicic acid (H₂SiF₆) operated at a current density 350 mA cm^− 2 at 25 °C and 1 min. The influence of H₂SiF₆ concentrations on the trivalent chromium electrodeposition was studied by the potentiodynamic technique. The phase structure and surface morphology of the deposited films were examined by using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The chemical composition of these thin films was determined by energy dispersive X-ray analysis (EDS) and X-ray photoelectron spectroscopy (XPS) analysis. The spectral reflectance in the visible light, for films coating was characterized. From the SEM analysis, it was found that the black chromium has nano lamellar morphology that leads to a strong dispersion level. The XRD results showed that chromium, chromium oxide and cobalt oxide are the main bulk chemical compounds in the films. However, from XPS analysis of these surfaces, it was possible to determine that the most external layers of the films are made of different kinds of chromium and cobalt compounds. The black chromium-cobalt alloy thin film has better optical properties to transform solar energy into thermal energy, and these properties remain practically constant even when heat treated to a high temperature, 400 °C for 24 h.     

Influence of heat treatment and gamma-rays irradiation on the structural and optical characterizations of nano-crystalline cobalt phthalocyanine thin films

Thin films of nano-crystalline cobalt phthalocyanine (CoPc) were prepared by thermal evaporation technique under high vacuum at room temperature and were identified by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The prepared films were divided into three groups for study; the first was the as deposited films, the second was heat treated under vacuum for 1 h at 630 K, and the third group was irradiated in gamma cell type ⁶⁰Co source in air at room temperature with total absorbed dose of 150 kGy. The optical properties for the three groups were investigated using spectrophotometric measurements of the transmittance and reflectance at normal incidence of light in the wavelength range from 200 to 2500 nm. The optical constants, refractive index, n, and absorption index, k, were calculated and found to be independent of film thickness in the measured film thickness range. The dispersion energy, E_d the oscillator energy, E₀ and the high frequency dielectric constant, ?_∞ of the three groups were obtained. The energy band model was applied and the types of the optical transitions responsible for optical absorption were found to be indirect allowed transition. The onset and optical energy gaps were calculated. Discussion of the obtained results and their comparison with the previously published data were also given.     

Structural and optical properties of electrodeposited ZnO thin films on conductive RuO2 oxides

ZnO thin films were grown on the 150 nm-thick RuO₂-coated SiO₂/Si substrates by electrochemical deposition in zinc nitrate aqueous solution with various electrolyte concentrations and deposition currents. Crystal orientation and surface structure of the electrodeposited ZnO thin films were characterized by X-ray diffraction (XRD) and scanning electron microscopy, respectively. The XRD results show the as-electrodeposited ZnO thin films on the RuO₂/SiO₂/Si substrates have mixed crystallographic orientations. The higher electrolyte concentration results in the ZnO thin films with a higher degree of c-axis orientation. Moreover, the use of an ultra-thin 5 nm-thick ZnO buffer layer on the RuO₂/SiO₂/Si substrate markedly improves the degree of preferential c-axis orientation of the electrodeposited ZnO crystalline. The subsequent annealing in vacuum at a low temperature of 300 °C reduces the possible hydrate species in the electrodeposited films. The electrodeposited ZnO thin films on the 5 nm-thick ZnO buffered RuO₂/SiO₂/Si substrates grown in 0.02 M electrolyte at −1.5 mA with a subsequent annealing in vacuum at 300 °C had the best structural and optical properties. The UV to visible emission intensity ratio of the film can reach 7.62.     

N, Fe and WO3 modified TiO2 for degradation of formaldehyde

Butyltitanate, ethanol and glacial acetic acid were chosen as titanium source, solvent and chelating agent, respectively, via a sol-gel method combined impregnation method to prepare N, Fe co-doped and WO₃ compounded photocatalyst TiO₂ powder. The synthesized products were characterized by X-ray diffraction (XRD), diffuse reflectance UV-Vis spectra (UV-DRS), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Photocatalytic degradation of formaldehyde was employed to investigate the catalytic activity. The results show that the degradation rate is 77.61% in 180 min under UV light irradiation when the concentration of N is fixed on, and the optimum proportioning ratio of n(Fe):n(W):n(Ti) is 0.5:2:100.     

Nanosphericals and nanobundles of ZnO: Synthesis and characterization

ZnO nanosphericals and nanobundles well dispersion have been synthesized using [(N,N′-bis(salicylaldehydo)ethylenediamine)zinc(II)]; [Zn(salen)] as precursor via two methods. Nanosphericals of ZnO has been prepared via thermal decomposition of [Zn(salen)] in the presence of oleylamine at 290 °C for 90 min. Also nanobundle of ZnO has been synthesized via thermolysis of [Zn(salen)] in the air at 500 °C for 5 h. The as-synthesized products were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and scanning electronic microscopy (SEM). The room temperature photoluminescence (PL) spectra of both nanostructures are dominated by the green emission attributed to the oxygen vacancy (V_O) related donor-acceptor transition. Presence of several infrared (IR) inactive vibrational modes in the Fourier transform infrared (FT-IR) absorption spectra of the samples indicates a breakdown of translational symmetry in the nanostructures induced by native defects.     

Decorating Mg/Fe oxide nanotubes with nitrogen-doped carbon nanotubes

Mg/Fe oxide nanotubes decorated with nitrogen-doped carbon nanotubes (CN_x) were fabricated by catalytic chemical vapor deposition of ethylenediamine on the outer surface of oxide nanotubes. Mg/Fe oxide nanotubes were prepared using a 3:1 molar precursor solution of Mg(NO₃)₂ and Fe(NO₃)₃ and anodic aluminum oxide as the substrate. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometer (VSM). The XRD pattern shows that the oxide nanotubes are made up of MgO and Fe₂O₃. TEM and SEM observations indicate the oxide nanotubes are arrayed roughly parallel to each other, and the outer surface of oxide nanotubes are decorated with CN_x. XPS results show the nitrogen-doped level in CN_x is about 7.3 at.%. Magnetic measurements with VSM demonstrate the saturated magnetization, remanence and coercivity of oxide nanotubes are obvious improved after being decorated with CN_x.     

Effect of nitrogen pressure on structure and optical properties of pulsed laser deposited BCN thin films

Amorphous boron carbon nitride (BCN) thin films were deposited on Si (100) and quartz substrates by laser ablation of a boron carbide (B₄C) target in nitrogen atmosphere. The effects of the nitrogen pre ssure (p_N2) on the film deposition rate, composition, structure and optical properties were investigated. The film deposition rate was measured by a surface profiler, which increased from 3.4 to 6.25 nm/min at elevated p_N2. Structure and composition of the films were investigated by X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared (FTIR) spectroscopy. FTIR and XPS analyses indicated that the as-deposited BCN films contained B-C, N-C and B-N chemical bonds, implying the formation of ternary BCN compounds. The nitrogen content in the films increased gradually and then saturated up to ∼ 26 at.% at 10 Pa p_N2. The optical band gap (E_g) increased from 3.78 to 3.92 eV with increasing p_N2 from 2 to 15 Pa. The evolution of E_g is in accordance with the change of film compositions and bonding states.     

磁过滤阴极弧法制备CrCN薄膜结构与组分研究

目的通过磁过滤阴极弧沉积技术制备质量优异的CrCN涂层。研究乙炔/氮气混合气体流量以及基底偏压对薄膜结构和成分的影响。方法采用磁过滤真空阴极弧沉积技术,在20~100 m L/min变化的乙炔/氮气混合气体流量参数下沉积CrCN复合薄膜。通过X射线衍射、场发射电子显微镜、扫描探针显微镜、X射线光电子能谱仪、透射电镜,对薄膜的物相结构和形貌进行分析。结果随着气体流量的增加,CrCN复合薄膜的晶粒逐渐减小最终向非晶化转变。TEM结果表明,在CrCN复合薄膜中有大量几纳米到十几纳米的纳米晶浸没在非晶成分中。SPM表明,随着基底偏压由–200 V增大到–150 V,CrCN薄膜的表面粗糙度Sa由0.345 nm上升至4.38 nm。XPS、TEM和XRD数据表明,薄膜中Cr元素主要以单质Cr、Cr N以及Cr3C2的形式存在。结论采用磁过滤真空阴极弧沉积技术制备的CrCN复合薄膜具有纳米晶-非晶镶嵌结构。该方法沉积的CrCN薄膜的表面粗糙度与基底负偏压有关。混合气体的流量变化对薄膜组分的变化几乎无影响。     

溅射功率对La-Ti/WS2 复合薄膜高温摩擦学行为的影响

高温条件下WS₂易于氧化生成WO3,导致WS₂固体润滑薄膜的摩擦学性能受到较大影响。为改善WS₂固体润滑薄膜在高温条件下的摩擦学性能,采用非平衡磁控溅射技术制备了共掺杂La-Ti/WS₂复合薄膜,研究了靶功率对磁控溅射La-Ti/WS₂复合薄膜结构和高温摩擦学性能的影响。利用扫描电镜(SEM)、X射线衍射仪(XRD)、纳米压痕仪和X射线光电子能谱仪(XPS)分析了薄膜微观形貌、成分、力学性能、微观结构。利用高温摩擦磨损试验机研究了复合薄膜的高温摩擦学性能。结果表明,高温环境下,靶功率为20W时La-Ti/WS₂复合薄膜表现出优异的摩擦学性能。此时,复合薄膜H/E值最大,摩擦系数最小,平均为0.012,磨损率最低为1.56×10^-8mm³/N·m,这主要归因于高温下摩擦界面产生的稀土氧化物,促使La-Ti/WS₂复合薄膜的摩擦磨损机制发生了改变,使得WS₂在高温受破坏的情...     

Structural, optical and chemical analysis of zinc sulfide thin film deposited by RF-mganetron sputtering and post deposition annealing

Zinc sulfide (ZnS) thin films were deposited by radio-frequency (RF) magnetron sputtering. The effects of the process parameters such as deposition time and RF-power, as well as of post deposition annealing under oxygen containing atmospheres, on the material properties of ZnS films have been investigated. X-ray diffraction analysis reveals out that the as-deposited ZnS films preferred (002) hexagonal wurtzite and (111) cubic zinc blend (111) at 28.60°, while a thicker ZnS film has additional hexagonal wurtzite (100), (110), and (200) planes coexisting with the preferred oriented-planes, suggesting that the thickness is dependent on the growth of ZnS. After annealing, ZnO phases were detected, indicating island-like grain growth on the surface of the ZnS film. By increasing the deposition time and the RF power, the optical band gap energy (E_g) of the ZnS film changes from 4.13 to 3.87 eV, indicating the presence of lower E_g with thicker ZnS film. The lower E_g (～3.27 eV) value of the annealed films is attributed to the ZnO transition. Unlike bulk ZnS material (Zn/S～1.08), deposited ZnS thin film has Zn-rich and S-deficient composition (Zn/S～1.28). However, the Zn/S ratio is closer to the ideal value when there is a longer deposition time or higher RF-power.     

Thermal stability of sol–gel p-type Al–N codoped ZnO films and electric properties of nanostructured ZnO homojunctions fabricated by spin-coating them on ZnO nanorods

The thermal stability of sol–gel p-type Al–N codoped ZnO films was investigated by high-resolution X-ray photoelectron spectroscopy (XPS). XPS revealed the chemical bonding states and solubility of N-related complex defects in the ZnO films. The concentrations of N_O and (NC)_O varied with annealing temperature, which led to the change in conduction between p-type and n-type. Variable-temperature Hall-effect measurement showed that N_O acted as a shallow acceptor, with its energy level locating at ～114 meV above the valance band maximum. Transmission electron microscopy confirmed the presence of undesired carbon clusters as a graphite state in the ZnO films. In order for Al–N codoped ZnO films to exhibit p-type conductivity, samples could only be annealed in a certain range of temperatures. A hybrid structure with nanostructured ZnO homojunctions was fabricated by spin-coating the p-type Al–N codoped ZnO film on an n-type ZnO nanorod array (ZNA). The hybrid nanostructure was demonstrated to possess rectification behavior characteristic of a p–n junction. The leakage current of the nanostructured ZnO homojunctions was smaller by a factor of 2 than that of the film-based ZnO homojunction at a reverse bias of 5 V. The p-type ZnO film/n-type ZNA structure can be applied as a versatile p–n optoelectronic device.     

Effect of Mg and Co co-doping on electrochemical properties of LiFePO4

LiFePO₄ co-doped with Mg²⁺ and Co⁴⁺ ions was synthesized by a solid state reaction method. The structure and electrochemical properties of the prepared LiFe_0.99Mg_0.005Co_0.005PO₄ were investigated by X-ray diffraction (XRD), galvanostatic charge-discharge experiment and cyclic voltammograms (CV). Specific discharge capacity of LiFePO₄ co-doped with Mg and Co ions reach 147.2 mA·h/g at 0.1C and 133.3 mA·h/g at 1C. The results of CV show that the reversibility of lithium extraction/insertion in LiFePO₄ can be promoted by (Mg²⁺, Co⁴⁺) multiple-ion doping.     

The photocatalytic activity of sprayed Zn1 − xMgxO thin films

ZnO has received much attention in the degradation and complete mineralization of environmental pollutants. For the purpose of increasing the photocatalytic efficiency of ZnO, Mg was doped into ZnO thin films.Zn_1 − xMg_xO thin films were prepared by spray pyrolysis method on glass substrates. The deposition temperature was 500 °C. Mg concentration was varied in the range of 0.0 to 0.3 in intervals of 0.05. The pure ZnO films were polycrystalline with preferred orientation (100). Zn_1 − xMg_xO becomes amorphous with increasing Mg concentration. The optical band gap of Zn_1 − xMg_xO changes from 3.26 to 3.59 eV with increasing Mg content. Also, the photocatalytic activity increased with Mg, and the film with x = 0.3 showed the best result.     

Synthesis, characterization and photocatalytic activity of NaNbO3/ZnO heterojunction photocatalysts

A series of NaNbO₃/ZnO heteronanostructures were synthesized with the hydrothermal method. Various characterization methods such as X-ray powder diffraction (XRD), scanning electronic microscope (SEM) and energy dispersive X-ray spectrometer (EDS), transmission electron microscope (TEM), X-ray photoelectron spectra (XPS) and diffuse reflectance spectra (DRS) were employed to investigate the structure, morphology and photocatalytic properties. The photocatalytic activity of the catalysts was evaluated by the degradation of methylene blue dye and the highest photocatalytic efficiency was observed when the content of NaNbO₃ was 10 wt.%. The photocatalytic mechanism of the heterojunction was also discussed. The effective transformation of the photoexcited electron and holes restricted the recombination of charges, which was regarded as the main reason of the high photocatalytic activity.     

钇、镉共掺杂氧化锌纳米粉体的合成及光学性能

为了研究能隙修改和发光强度之间的关系,通过化学共沉淀法制备钇、镉共掺杂的氧化锌纳米粉体。采用XRD、XPS及PL对样品的晶体结构和光学性能进行研究。通过对钇、镉离子对氧化锌光学性能影响的研究发现,钇的掺入能够有效地增强氧化锌的紫外发光,钇、镉共掺杂在增强发光的同时,还使得氧化锌的带隙窄化,使得紫外发光红移,从而使得样品的室温光致发光图谱呈现出增强的紫光发射。该材料有望应用在制备光电器件方面。