Micromorphology and nanomechanical characteristics of sputtered aluminum thin films

Micromorphology and nanoindentation properties of sputtered aluminum thin films are presented. The field emission scanning electron microscope, atomic force microscopy (AFM) and nanoindentation results are presented for films prepared at a substrate temperature ranging between 44.5 °C and 100 °C. A multifractal approach on the microstructure is presented to comprehend the micromorphology of the films. The roughness decreases, whereas fractal dimension increases as the temperature increases. The hardness and Young's modulus do not exhibit any predictable trend. Hardness and Young's modulus exhibit a linear relationship.     

AFM nanopatterning of transition metal oxide thin films

In this paper we show diverse methods for patterning transition metal oxide (TMO) thin films by Local Anodic Oxidation (LAO) using an Atomic Force Microscope (AFM). At first, direct lithography by current-controlled LAO of TMO thin films and selective wet etching is presented. For insulating films or those whose AFM patterns cannot be selectively removed by wet etching, fabrication of nanomasks is required; thus, the fabrication of Molybdenum and TMO nanomasks is reported. As a further development, we show the AFM fabrication of Mo/poly(methylmethacrylate) (PMMA) nanomasks through multistep processes combining LAO of Mo and dry etching of PMMA. Detailed discussions and comparisons between these methods are presented.     

Nanostructured copper and copper oxide thin films fabricated by hydrothermal treatment of copper hydroxide nitrate

Metallic copper and copper oxide thin films were fabricated on surface of glass slide substrates. Copper oxide thin films were prepared by a hydrothermal method using an α-phase layered hydroxide, copper hydroxide nitrate as a precursor. Morphology, thickness and crystallite size of the obtained copper oxide thin films changed by changing the time of hydrothermal treatment. Accordingly, the copper oxide thin films showed various water contact angles and optical band gaps. As, the optical band gap of the nanostructured copper oxide thin films increased with an increase in hydrothermal time from 1.85 to 2.95 eV. Moreover, the water contact angles changed from 16.4 to 38.8° by changing the hydrothermal time. By a reductive hydrothermal-treatment route, the copper oxide thin film was reduced to metallic copper thin film without any particle growth.     

Mechanical characterization of single crystal silicon and UV-LIGA nickel thin films using tensile tester operated in AFM

This paper describes the mechanical characteristics of microscale single crystal silicon (SCS) and UV‐LIGA nickel (Ni) films used for microelectromechanical systems (MEMS). A compact tensile tester, operated in an atomic force microscope (AFM), was developed for accurate evaluation of Young's modulus, tensile strain and tensile strength of microscale SCS and UV‐LIGA Ni specimens. SCS specimens with nominal dimensions of 20 μm in thickness, 50 μm in width and 600 μm in length were prepared by a conventional photolithography and etching process. UV‐LIGA Ni specimens, with a thickness of 15 μm, a width of 50 μm and a length of 600 μm in nominal dimensions, were also fabricated by electroplating using a UV thick photoresist mould. All specimens have line patterns on their specimen gauge section to measure axial elongation under tensile loading. The SCS specimens showed a linear stress–strain response and fractured in a brittle manner, whereas the UV‐LIGA Ni specimens showed elastic–inelastic deformation behaviour. Young's modulus of SCS and UV‐LIGA Ni specimens obtained from tensile tests averaged 169.2 GPa and 183.6 GPa, respectively, close to those of bulk materials. However, the tensile strength of both materials showed a larger value than the bulk materials: 1.47 GPa for the SCS and 0.98 GPa for the Ni specimens. Yield stress and breaking elongation of UV‐LIGA Ni specimens were also quite different from those of the bulk Ni because of the specimen size effect on inelastic properties.     

Preparation and characterization of nanostructured copper bismuth diselenide thin films from a chemical route

Thin films of copper bismuth diselenide were prepared by chemical bath deposition technique ontoglass substrate below 60°C. The deposition parameters such as time, temperature of deposition and pH of the solution, were optimized. The set of films having different elemental compositions was prepared by varying Cu/Bi ratio from 0·13–1·74. Studies on structure, composition, morphology, optical absorption and electrical conductivity of the films were carried out and discussed. Characterization includes X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray analysis (EDAX), absorption spectroscopy, and electrical conductivity. The results are discussed and interpreted.     

Nanocrystalline copper selenide thin films by chemical spray pyrolysis

Thin films of copper selenide were deposited onto amorphous glass substrates at various substrate temperatures by computerized spray pyrolysis technique. The as deposited copper selenide thin films were used to study a wide range of characteristics including structural, surface morphological, optical and electrical, Hall Effect and thermo-electrical properties. X-ray diffraction study reveals that the films are polycrystalline in nature with hexagonal (mineral klockmannite) crystal structure irrespective of the substrate temperature. The crystalline size is found to be in the range of 23–28 nm. The SEM study reveals that the grains are uniform with uneven spherically shaped and spread over the entire surface of the substrates. EDAX analysis confirmed the nearly stoichiometric deposition of the film at 350 °C. The direct band gap values are found to be in the range 2.29–2.36 eV depending on the substrate temperature. The Hall Effect study reveals that the films exhibit p-type conductivity. The values of carrier concentration and mobility for the film are found to be 5.02 × 10¹⁷ cm^?3 and 5.19 × 10^?3 cm² V^?1 s^?1; respectively for film deposited at 350 °C.     

Reactive DC magnetron sputter deposited copper nitride nano-crystalline thin films: Growth and characterization

CuN_x thin films were grown by reactive DC magnetron sputtering and their structural, morphological, optical and electrical properties were evaluated. This study provides insight into the importance of substrate temperature and nitrogen content on the characteristic of CuN_x films. Phase analysis and structural properties of these films were identified by X-ray diffraction (XRD) technique. XRD results showed that the CuN_x films were single phase and polycrystalline with mixed orientation. Nitrogen excess accommodates in vacant interstitial sites of cubic anti-ReO₃ crystal structure of CuN_x and exhibits a solid solubility. The variation of surface morphology, studied by scanning electron microscope (SEM), shows suppression of the pyramidal-like grain growth by N richness. Optical study were performed by UV-Vis-near IR transmittance spectroscopy. Film thickness, refractive index and extinction coefficient were extracted from the measured transmittance using a reversed engineering method. Absorption coefficient and electrical resistivity indicate that the CuN_x films present extrinsic semiconducting behavior with an indirect optical band gap between 1.19 and 1.44 eV. To confirm the optical band gap energy, a first principle calculation was performed and compared with the measured data.     

Preparation and characterization of copper(II) oxide thin films grown by a novel spray pyrolysis method

A novel spray pyrolysis reactor was used to prepare thin films of CuO on silica substrates. The resulting films were characterized by x-ray diffraction, electron microscopy, optical and electrical measurements. The films were single phase, homogeneous, and uniform.     

Ellipsometry of thin films of copper phthalocyanine

Ellipsometric measurements have provided qualitative information on the optical properties of CuPC films deposited on a thin gold layer substrate. Detailed interpretation was complicated by variations in the density of the deposited layers and the surface roughness of the substrate. Films less than 100 nm thick can be satisfactory represented by a single homogeneous isotropic layer. Thicker films appear to be equivalent to an isotropic inner layer and an anisotropic outer layer, where the latter results from bulk deposition of CuPC with the molecules in a predominant orientation to the surface. Reasonable agreement has been obtained between film thicknesses measured by weighing and by ellipsometry, assuming a single homogeneous anisotropic film for thickness in excess of 150 nm.     

Preparation and characterization of PLZT thin films by sol-gel processing

The effect of acid catalysts on the sol-gel preparation of ferroelectric lead lanthanum zirconium titanate (PLZT) thin films was studied. High quality thin films were successfully produced by using suitable amounts of the drying control chemical additive formamide and also catalyst acids during the sol-gel processing followed by various annealing conditions. The dielectric constants of the PLZT (8/65/35) thin films produced in this study varied between 540 (100 kHz) for a film annealed at 600 °C for 30 mins to a maximum 870 °C (1 kHz), 700 (100 kHz) for a film annealed at 650 °C for 20 mins.     

Diffusion of copper in thin TiN films

The diffusivity of copper in thin TiN layers was determined in specimens prepared by r.f. sputtering a copper (80 nm) layer onto a TiN (200 nm) layer on sapphire and silicon substrates. Specimens were isothermally heat treated at 608, 635 and 700 °C at pressures lower than 2 × 10^?6 Pa; they were compositionally analyzed by Rutherford backscattering spectroscopy and Auger sputter profiling; and they were microstructurally characterized by transmission electron microscopy and electron diffraction. The diffusivity D = 9 × 10⁷cm²s^?1exp(?427 kJmol^?1/RT) from 608 to 700 °C. The mechanisms of copper diffusion were not bulk processes, but they were probably processes involving primarily grain boundaries in the TiN. This very low diffusivity at these temperatures makes TiN/Cu an excellent candidate for a high temperature metallization for silicon solar concentrator cells.     

Structural characterization and porosity analysis in self-supported porous alumina-silica thin films

In this study, alumina, silica and alumina-silica binary (36% mol silica) thin films are synthesized using the sol-gel technique. These form the basis for future gas separation membranes. The characterization of the synthesized oxides was performed using nitrogen physisorption, X-ray diffraction (XRD), Doppler-broadening measurements on the 511 keV annihilation photon peak, together with 3γ/2γ analysis, and Fourier transform infrared spectroscopy (FTIR) of adsorbed CO. It is found that silica is microporous, γ-alumina is mesoporous, and the binary material shows fingerprints of both the meso- and microporous nature of its constituents as well as of the respective crystal structures. These results open the possibility to also investigate thin supported porous films (a few microns thick), and especially the setting and drying aspects on porous supports for membrane production, using the positron annihilation technique.     

Single-step electrochemical nanolithography of metal thin films by localized etching with an AFM tip

This work introduces electrochemical nanolithography (ENL), a single-step method in which a metal thin film is locally etched without application of a mask on a 100?nm length scale with an electrochemical atomic force microscope (AFM). The method requires the application of ultra-short voltage pulses on the tip (nanosecond range duration, 2-4?V amplitude), while both the sample and the metalized tip are under independent potentiostatic control for full control of interface reactions in an AFM electrochemical cell. It is demonstrated that Cu films as well as Co and Cu/Co sandwich magnetic films can be patterned if negative voltage pulses are applied to the tip. This method also applies to films deposited on an insulating substrate. Moreover the lateral dimension of lithographed structures is tunable, from a few micrometers down to 150?nm, by appropriate choice of ENL conditions. Simulation of the dissolution process is discussed.     

Structural characterization of lead sulfide thin films by means of X-ray line profile analysis

X-ray diffraction patterns of chemically deposited lead sulphide thin films have been recorded and X-ray line profile analysis studies have been carried out. The lattice parameter, crystallite size, average internal stress and microstrain in the film are calculated and correlated with molarities of the solutions. Both size and strain are found to contribute towards the broadening of X-ray diffraction line. The values of the crystallite size are found to be within the range from 22–33 nm and the values of strain to be within the range from 1·0 × 10⁻³–2·5 × 10⁻³.     

Optical characterization of thin chalcogenide films by multiple-angle-of-incidence ellipsometry

Optical properties of thin chalcogenide films from the systems As-S(Se) and As-S-Se were investigated as a function of the film composition, film thickness and conditions of illumination by light using multiple-angle-of-incidence ellipsometry. Thin films were deposited by thermal evaporation and exposed to white light (halogen lamp) and to monochromatic light from Ar⁺ — (λ = 488, 514 nm) and He-Ne- (λ = 632.8 nm) lasers. The ellipsometric measurements were carried out at three different angles of light incidence in the interval 45-55°, at λ = 632.8 nm. An isotropic absorbing layer model was applied for calculation of the optical constants (refractive index, n and extinction coefficient, k) and film thickness, d. The homogeneity of the films was checked and verified by applying single-angle calculations at different angles. It was shown that the refractive index, n of As-S-Se films is independent of film thickness in the range of 50 to 1000 nm and its values varied from 2.45 to 3.05 for thin layers with composition As₂S₃ and As₂Se₃, respectively. The effect of increasing in the refractive index was observed after exposure to light which is related to the process of photodarkening in arsenic containing layers. The viability of the method for determining the optical constants of very thin chalcogenide films with a high accuracy was confirmed.     

Structural characterization of thin ZnS films by X-ray diffraction

Structural properties of electroluminescent ZnS: Mn thin films grown by atomic layer epitaxy, which emit yellow light with an external efficiency as high as 2%, are investigated. The films grown at 500°C have a strong preferred orientation: one-half of the 00·1 plane normals are aligned within 7° from the normal of the glass substrate. The length of coherently diffracting domains (crystallite size) in the direction of the normal obtained from the Fourier analysis of a line profile ranges from 30 to 160 nm. The average relative strain in the same direction is calculated to be 10^?3. The estimated dislocation density is about 10¹⁰ cm^?2.     

Low temperature oxidation of copper alloys—AEM and AFM characterization

Oxidation kinetics and oxide structures of three polycrystalline copper grades at different temperatures were studied by analytical transmission electron microscopy (AEM) and atomic force microscopy (AFM). The copper samples were oxidized in air at 200 and 350 °C for 1–1,100 min. AEM and AFM studies indicated that alloying and increase of temperature, accelerated oxidation. At 200 °C local oxidation was observed in the unalloyed copper samples while a uniform oxide layer formed on the alloyed coppers. At 350 °C a uniform oxide layer formed on all copper samples. The oxide structure was nanocrystalline cubic Cu₂O after all oxidation treatments at 200 °C and after 5 min oxidation at 350 °C. After 25 and 100 min oxidation at 350 °C the crystal size of copper oxide had grown and the oxide structure was monoclinic CuO.     

Photothermal characterization of thin films and coatings

The principles of non-destructive, non-contact characterization of coatings by means of photothermal measuring techniques are briefly explained. A method of quantitative interpretation is presented, which relies on the relative extrema of the calibrated thermal wave phase lags measured as a function of the heating modulation frequency for coatings deposited by reactive magnetron sputtering. The application potential of this interpretation method with respect to the on-line control of coating deposition processes is discussed.     

Texture and hillocking in sputter-deposited copper thin films

Copper thin films have been deposited by magnetron sputtering under a wide variety of conditions. In nearly all cases, (1 1 1) texture is predominant, although its extent varies with the conditions. Greater texture appears to be associated with abnormal grain growth during deposition. For films deposited on novel amorphous SiN _x , barriers made by in-situ nitriding of SiO₂, the texture is significantly weaker than on conventional Ta or TaN underlayers. Pronounced thermal hillocking is observed. As has been found for other ccp metals, strong (1 1 1) texture suppresses the tendency to hillocking.