One-Dimensional Photonic Crystals with Nonbranched Pores Prepared via Phosphorous Acid Anodizing of Aluminium

One-dimensional photonic crystals (1D PhCs) obtained by aluminium anodizing under oscillating conditions are promising materials with structure-dependent optical properties. Electrolytes based on sulphuric, oxalic, and selenic acids have been utilized for the preparation of anodic aluminium oxide (AAO) 1D PhCs with sub-100-nm pore diameter. AAO films with larger pores can be obtained by anodizing in phosphorous acid at high voltages. Here, for the first time, anodizing in phosphorous acid is applied for the preparation of AAO 1D PhCs with nonbranched macropores. The sine wave profile of anodizing voltage in the 135–165 V range produces straight pores, whose diameter is above 100 nm and alternates periodically in size. The pore diameter modulation period linearly increases with the charge density by a factor of 599 ± 15 nm·cm2·C−1. The position of the photonic band gap is controlled precisely in the 0.63–1.96 µm range, and the effective refractive index of AAO 1D PhCs is 1.58 ± 0.05

Long-Term Operational Stability of Ta/Pt Thin-Film Microheaters: Impact of the Ta Adhesion Layer

Microheaters with long-term stability are crucial for the development of a variety of microelectronic devices operated at high temperatures. Structured Ta/Pt bilayers, in which the Ta sublayer ensures high adhesion of the Pt resistive layer, are widely used to create microheaters. Herein, a comprehensive study of the microstructure of Ta/Pt films using high-resolution transmission electron microscopy with local elemental analysis reveals the twofold nature of Ta after annealing. The main fraction of Ta persists in the form of tantalum oxide between the Pt resistive layer and the alumina substrate. Such a sublayer hampers Pt recrystallization and grain growth in bilayered Ta/Pt films in comparison with pure Pt films. Tantalum is also observed inside the Pt grains as individual Ta nanoparticles, but their volume fraction is only about 2%. Microheaters based on the 10 nm Ta/90 nm Pt bilayers after pre-annealing exhibit long-term stability with low resistance drift at 500 °C (less than 3%/month)

Towards High-Temperature MEMS: Two-Step Annealing Suppressed Recrystallization in Thin Multilayer Pt-Rh/Zr Films

Platinum-based thin films are widely used to create microelectronic devices operating at temperatures above 500 °C. One of the most effective ways to increase the high-temperature stability of platinum-based films involves incorporating refractory metal oxides (e.g., ZrO2, HfO2). In such structures, refractory oxide is located along the metal grain boundaries and hinders the mobility of Pt atoms. However, the effect of annealing conditions on the morphology and functional properties of such multiphase systems is rarely studied. Here, we show that the two-step annealing of 250-nm-thick Pt-Rh/Zr multilayer films instead of the widely used isothermal annealing leads to a more uniform film morphology without voids and hillocks. The composition and morphology of as-deposited and annealed films were investigated using X-ray diffraction and scanning electron microscopy, combined with energy-dispersive X-ray spectroscopy. At the first annealing step at 450 °C, zirconium oxidation was observed. The second high-temperature annealing at 800–1000 °C resulted in the recrystallization of the Pt-Rh alloy. In comparison to the one-step annealing of Pt-Rh and Pt-Rh/Zr films, after two-step annealing, the metal phase in the Pt-Rh/Zr films has a smaller grain size and a less pronounced texture in the direction, manifesting enhanced high-temperature stability. After two-step annealing at 450/900 °C, the Pt-Rh/Zr thin film possessed a grain size of 60 ± 27 nm and a resistivity of 17 × 10−6 Ω·m. The proposed annealing protocol can be used to create thin-film MEMS devices for operation at elevated temperatures, e.g., microheater-based gas sensors

Crystallography-Induced Correlations in Pore Ordering of Anodic Alumina Films

A crystallographic approach to tailoring the morphology and ordering degree of the porous structure of alumina films obtained by anodization of single-crystalline aluminum is discussed. The examination of porous structure of anodic alumina films formed on low-index and vicinal planes of Al single crystals under self-ordering conditions by high-resolution small-angle X-ray scattering revealed the existence of two pore growth directions on vicinal facets. The inclination of channels from the normal to the metal surface is explained by the competitive impact of electromigration driving force and the crystallographic anisotropy of the substrate. It was also shown that pores growing in different directions during anodization retain hexagonal domains with various in-plane orientations. These results for the first time demonstrate the strong correlations between the longitudinal alignment and in-plane packing options of pores in anodic alumina films

High-resolution SAXS setup with tuneable resolution in direct and reciprocal space : A new tool to study ordered nanostructures

A novel compact small-angle X-ray scattering (SAXS) setup with tuneable resolution in both direct and reciprocal space has been designed and tested for the study of nanostructured materials with a hierarchical structure. The setup exploits a set of compound refractive lenses that focus the X-ray beam at the detector position. Anodic alumina membranes with a self-ordered porous structure were chosen as test samples. The setup allows patterns to be collected with a minimum scattering vector value of 0.001 14;nm-1 and gives the possibility for an easy continuous switch between taking high-resolution statistically averaged diffraction data of macroscopically large sample volumes and lower-resolution diffraction on a small single domain of the anodic aluminium oxide film. It is revealed that the pores are longitudinal and their ordering within each domain tends towards the ideal hexagonal structure, whereas the in-plane orientation of the pore arrays changes from domain to domain. The possible advantages and disadvantages of the proposed compact SAXS scheme are discussed

High-resolution SAXS setup with tuneable resolution in direct and reciprocal space: a new tool to study ordered nanostructures

A novel compact small-angle X-ray scattering (SAXS) setup with tuneable resolution in both direct and reciprocal space has been designed and tested for the study of nanostructured materials with a hierarchical structure. The setup exploits a set of compound refractive lenses that focus the X-ray beam at the detector position. Anodic alumina membranes with a self-ordered porous structure were chosen as test samples. The setup allows patterns to be collected with a minimum scattering vector value of 0.001 14;nm-1 and gives the possibility for an easy continuous switch between taking high-resolution statistically averaged diffraction data of macroscopically large sample volumes and lower-resolution diffraction on a small single domain of the anodic aluminium oxide film. It is revealed that the pores are longitudinal and their ordering within each domain tends towards the ideal hexagonal structure, whereas the in-plane orientation of the pore arrays changes from domain to domain. The possible advantages and disadvantages of the proposed compact SAXS scheme are discussed

Growth of porous anodic alumina on low-index surfaces of Al single crystals

The pseudoepitaxial growth of amorphous anodic alumina with ordered porous structure within single crystal grains of aluminum substrates is an amazing feature of the self-organization process, which occurs during anodization. Here, we used single crystal Al(100), Al(110), and Al(111) substrates to inspect the effect of aluminum crystallography on anodization rates and the morphology of the resulting alumina films grown under different anodization conditions. The difference in the kinetics of porous film growth on various substrates is described in terms of the activation barrier of aluminum atom release from the metal surface to the oxide layer. Scanning electron microscopy and small-angle X-ray scattering are applied for quantitative characterization of different kinds of ordering in anodic alumina films. The highest number of straight channels was found in porous anodic alumina grown on Al(100) substrates, whereas Al(111) was proved to induce the best orientational order in anodic alumina with the formation of the single-domain-like structures. Based on the obtained results, possible pathways for crystallographic control of the anodic alumina porous structure for different practical applications are discussed

High-resolution SAXS setup with tuneable resolution in direct and reciprocal space:a new tool to study ordered nanostructures

\u3cp\u3eA novel compact small-angle X-ray scattering (SAXS) setup with tuneable resolution in both direct and reciprocal space has been designed and tested for the study of nanostructured materials with a hierarchical structure. The setup exploits a set of compound refractive lenses that focus the X-ray beam at the detector position. Anodic alumina membranes with a self-ordered porous structure were chosen as test samples. The setup allows patterns to be collected with a minimum scattering vector value of 0.001 14;nm\u3csup\u3e-1\u3c/sup\u3e and gives the possibility for an easy continuous switch between taking high-resolution statistically averaged diffraction data of macroscopically large sample volumes and lower-resolution diffraction on a small single domain of the anodic aluminium oxide film. It is revealed that the pores are longitudinal and their ordering within each domain tends towards the ideal hexagonal structure, whereas the in-plane orientation of the pore arrays changes from domain to domain. The possible advantages and disadvantages of the proposed compact SAXS scheme are discussed.\u3c/p\u3

Growth of Porous Anodic Alumina on Low-Index Surfaces of Al Single Crystals

The pseudoepitaxial growth of amorphous anodic alumina with ordered porous structure within single crystal grains of aluminum substrates is an amazing feature of the self-organization process, which occurs during anodization. Here, we used single crystal Al(100), Al(110), and Al(111) substrates to inspect the effect of aluminum crystallography on anodization rates and the morphology of the resulting alumina films grown under different anodization conditions. The difference in the kinetics of porous film growth on various substrates is described in terms of the activation barrier of aluminum atom release from the metal surface to the oxide layer. Scanning electron microscopy and small-angle X-ray scattering are applied for quantitative characterization of different kinds of ordering in anodic alumina films. The highest number of straight channels was found in porous anodic alumina grown on Al(100) substrates, whereas Al(111) was proved to induce the best orientational order in anodic alumina with the formation of the single-domain-like structures. Based on the obtained results, possible pathways for crystallographic control of the anodic alumina porous structure for different practical applications are discussed

Nd_2−xSr_xNiO₄ Solid Solutions: Synthesis, Structure and Enhanced Catalytic Properties of Their Reduction Products in the Dry Reforming of Methane

Solid solutions Nd2−xSrxNiO4±δ (x = 0, 0.5, 1, 1.2, 1.4) with a K2NiF4 structure can be obtained from freeze-dried precursors. The end members of this series can be obtained at T ≥ 1000 °C only, while complex oxides with x = 1; 1.5 are formed at T ≥ 700 °C. Thermal analysis revealed the two stages of Nd2−xSrxNiO4±δ thermal reduction in a 10%H2/Ar gas mixture that was completed at 900 °C. For x 1 revealed the outstanding catalytic activity and selectivity in the dry reforming of the methane (DRM) reaction at 800 °C with CH4 conversion close to the thermodynamic values. The appearance of two different maxima of the catalytic properties of Ni/(Nd2O3,SrCO3) nanocomposites could be affiliated with the domination of the positive contributions of Nd2O3 and SrCO3, respectively