Structure and mechanical properties of titanium nitride/carbon nitride multilayers

The structure and mechanical properties of the multilayers consisting of 5-73 nm thick titanium nitride (TiN) and 4.6 nm thick carbon nitride (CN) have been investigated. It has been found that the CN layers are amorphous and the TiN layers thinner than 17 nm are amorphous. The TiN layers become crystallized as the thickness is increased to 30 nm or thicker. The hardness from the composite response of the multilayered films and their substrates determined using continuous stiff measurement is smaller than the film-only hardness (without substrate effects) calculated using Bhattacharya-Nix empirical equation. The hardness increases with raising the thickness of TiN layers. With the crystallization of the TiN layer, the multilayers become even harder than that calculated based on the rule of mixtures. However, no enhancement in hardness has been observed when the TiN layers are amorphous.     

TiCN/TiNbCN multilayer coatings with enhanced mechanical properties

Enhancement of mechanical properties by using a TiCN/TiNbCN multilayered system with different bilayer periods (Λ) and bilayer numbers (n) via magnetron sputtering technique was studied in this work. The coatings were characterized in terms of structural, chemical, morphological and mechanical properties by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nanoindentation. Results of the X-ray analysis showed reflections associated to FCC (1 1 1) crystal structure for TiCN/TiNbCN films. AFM analysis revealed a reduction of grain size and roughness when the bilayer number is increased and the bilayer period is decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 15 nm (n = 200), yielding the highest hardness (42 GPa) and elastic modulus (408 GPa). The values for the hardness and elastic modulus are 1.6 and 1.3 times greater than the coating with n = 1, respectively. The enhancement effects in multilayer coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain the increase in hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayers taking into account the thickness reduction at individual single layers that make the multilayered system. The Hall-Petch model based on dislocation motion within layers and across layer interfaces, has been successfully applied to multilayers to explain this hardness enhancement.     

Enhancement of surface mechanical properties by using TiN[BCN/BN]n/c-BN multilayer system

The aim of this work is to improve the mechanical properties of AISI 4140 steel substrates by using a TiN[BCN/BN]_n/c-BN multilayer system as a protective coating. TiN[BCN/BN]_n/c-BN multilayered coatings via reactive r.f. magnetron sputtering technique were grown, systematically varying the length period (Λ) and the number of bilayers (n) because one bilayer (n = 1) represents two different layers (t_BCN + t_BN), thus the total thickness of the coating and all other growth parameters were maintained constant. The coatings were characterized by Fourier transform infrared spectroscopy showing bands associated with h-BN bonds and c-BN stretching vibrations centered at 1400 cm⁻¹ and 1100 cm⁻¹, respectively. Coating composition and multilayer modulation were studied via secondary ion mass spectroscopy. Atomic force microscopy analysis revealed a reduction in grain size and roughness when the bilayer number (n) increased and the bilayer period decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 80 nm (n = 25), yielding the relative highest hardness (∼30 GPa) and elastic modulus (230 GPa). The values for the hardness and elastic modulus are 1.5 and 1.7 times greater than the coating with n = 1, respectively. The enhancement effects in multilayered coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain increased hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayered coatings taking into account the thickness reduction at individual single layers that make up the multilayered system. The Hall-Petch model based on dislocation motion within layered and across layer interfaces has been successfully applied to multilayered coatings to explain this hardness enhancement.     

Early stages of laser mixing process in Sb/Ge multilayer thin films

The onset of mixing at the interfaces between Sb and Ge in thin multilayered films containing two or four layers has been studied. The films were irradiated with nanosecond laser pulses in order to trigger mixing, and in situ reflectivity measurements were used to follow the transformation in real-time. Cross sectional transmission electron microscopy analysis was used to study both the structure and the composition profile before and after irradiation.A threshold irradiation energy exists for the onset of mixing, below which roughening of the interface between the layers is observed, together with recrystallization of the surface Sb layer following melting. The results are consistent with a melting/diffusion process which is inhomogeneously nucleated at the interface between the top Sb and Ge layers. Once mixing is initiated an amorphous Sb-Ge layer of constant thickness is formed, corresponding to mixing along a well defined planar melt front. Voids are observed at the former Sb/Ge interface, which may be related to interfacial stress in the as-grown configuration.     

Ferrimagnetic resonance spectra of magnetic bubble films at low microwave frequencies

Magnetic bubble films exhibit a number of ferrimagnetic resonance modes due to the spatial variation of the anisotropy. The resonance frequencies have been measured as a function of the applied bias fieldH ₀. In the lower field range the magnetization of the transient layer, which has negative anisotropy, is not yet parallel toH ₀. In this range the resonance frequencies are shifted to higher values due to pinning effects. In films grown by the vertical dipping method an additional layer on top of the transient layer is observed within which the magnetization rotates from the direction in the transient layer to that of the bulk of the film. In films grown by horizontal dipping no such layer could be detected. Each ferrimagnetic resonance mode excites transverse elastic waves in the film due to the magnetoelastic interaction and thus gives rise to elastic resonances of the whole crystal, film and substrate. These elastic resonances lead to a fine-structure of the ferrimagnetic resonances. The observed fine-structure vanishes periodically with frequency and from this behaviour the thickness of the magnetic film and of the transient layer has been determined.     

Study of Tb/Fe multilayers by temperature-dependent CEMS

A comparative study is accomplished in the domain where iron layers are amorphous. The dependence of the magnetic structure of Tb/Fe multilayered films on temperature have been investigated by Mössbauer spectrometry. When the iron layer is thinner than 2.3 nm, the average hyperfine field at the iron site remains nearly constant at 4.2 K, while it decreases strongly for iron thickness higher than 1.5 nm at room temperature. This decrease of H is due to the decrease of the Curie temperature, which can be explained from the structure of iron layers.     

Microhardness of condensation polymers and copolymers. 1. Coreactive blends of polyethylene terephthalate and polycarbonates

The microhardness of coreactive blends of polyethylene terephthalate (PET) and bisphenol A polycarbonate (PC) was investigated over the whole range of compositions. The occurrence of one single glass transition temperature (T _g) step in the differential scanning calorimetry (DSC) curves indicated that intensive chemical interactions had taken place during melt blending, resulting in formation of copolycondensates with dominating random sequential order. The parallel decrease of microhardness (H) and of T_g with increasing PET content in the blends has been ascribed to the formation of new copolymer molecules enriched in the component characterized by lower H and T _g values. It is emphasized that such noncrystallizable copolymers offer the possibility to evaluate the intrinsic contribution of the repeating units to the H and T _g characteristics of copolymers with various compositions and sequential orders.     

Preparation and mechanical properties of layers made of recombinant spider silk proteins and silk from silk worm

Layers of recombinant spider silks and native silks from silk worms were prepared by spin-coating and casting of various solutions. FT-IR spectra were recorded to investigate the influence of the different mechanical stress occurring during the preparation of the silk layers. The solubility of the recombinant spider silk proteins SO1-ELP, C16, AQ24NR3, and of the silk fibroin from Bombyx mori were investigated in hexafluorisopropanol, ionic liquids and concentrated salt solutions. The morphology and thickness of the layers were determined by Atomic Force Microscopy (AFM) or with a profilometer. The mechanical behaviour was investigated by acoustic impedance analysis by using a quartz crystal microbalance (QCMB) as well as by microindentation. The density of silk layers (d<300 nm) was determined based on AFM and QCMB measurements. At silk layers thicker than 300 nm significant changes of the half-band-half width can be correlated with increasing energy dissipation. Microhardness measurements demonstrate that recombinant spider silk and sericine-free Bombyx mori silk layers achieve higher elastic penetration modules E_EP and Martens hardness values H_M than those of polyethylenterephthalate (PET) and polyetherimide (PEI) foils.     

2-2型磁电复合薄膜CoFe2O4/Pb(Zr0.53Ti0.47)O3静磁耦合

运用溶胶-凝胶法在Pt/Ti/SiO₂/Si基片上旋涂制备了2-2型CoFe₂O₄/Pb(Zr_0.53Ti_0.47)O₃磁电复合薄膜．制备的磁电薄膜结构为基片/PZT/CFO/PZT*/CFO/PZT,通过改变中间层PZT*溶胶的浓度,改变磁性层间距以及静磁耦合的大小．SEM结果表明,复合薄膜结构致密,呈现出界面清晰平整的多层结构．制备的复合薄膜具有较好的铁电与铁磁性能．实验还研究了静磁耦合对薄膜磁电性能的影响,结果表明,随着复合薄膜磁性层间距的减小,静磁耦合效应的增加,磁电电压系数有逐渐增大的趋势.     

Domain structure of double layer single crystal films of iron

The domain structures of multilayered films consisting of mutually parallel single crystal (001) Fe layers and an LiF intermediate layer were studied by Lorentz microscopy. Magnetic flux transitions from layer to layer and formation of extraordinary domain walls were observed in systems with magnetic layers approximately equal in thickness. The effect of the adjacent layer on the 180° wall structure was observed.Died November 3rd, 1969.     

Ti-Si-N复合膜的界面相研究

为了揭示Ti_Si_N复合膜中Si₃N₄界面相的存在方式及其对薄膜力学 性能的影响 ，采用x射线衍射仪、高分辨透射电子显微镜、俄歇电子能谱仪和显微硬度仪对比研究了磁 控溅射Ti_Si_N复合膜和TiN/Si₃N₄多层膜的微结构和力学性能. 实 验结果表明 ，Ti_Si_N复合膜均形成了Si₃N₄界面相包裹TiN纳米晶粒的微结构. 其中低Si 含量的Ti_Si_N复合膜中Si₃N₄界面相的厚度小于1nm，且以晶体态 存在，薄膜 呈现高硬度. 而高Si含量的Ti_Si_N复合膜中的Si₃N₄界面相以非晶 态存在，薄 膜的硬度也相应降低. 显然，Ti_Si_N复合膜中Si₃N₄界面相以晶体 态形式存在 是薄膜获得高硬度的重要微结构特征，其强化机制可能与多层膜的超硬效应是相同的. 关键词： Ti－Si－N复合膜 界面相 微结构 超硬效应     

Dynamics of phase formation in multilayer Ti-Al nanofilms upon heating

Structural transformations in multilayer Ti-Al films (layer thickness from 4 to 500 nm, number of layers up to 4440, total foil thickness ∼18 μm) upon slow heating have been studied by time-resolved synchrotron radiation diffraction. Some specific features of heterogeneous reactions and the sequence of phase formation in multilayer samples during the interaction of interaction between layer components have been determined as functions of the single layer thickness. Original Russian Text ? I.Yu. Yagubova, A.E. Grigoryan, A.S. Rogachev, M.R. Sharafutdinov, B.P. Tolochko, P.A. Tsygankov, A.N. Nosyrev, 2007, published in Izvestiya Rossiiskoi Akademii Nauk. Seriya Fizicheskaya, 2007, Vol. 71, No. 2, pp. 278–279.     

A transmission electron microscopy study of the deformation behavior underneath nanoindents in nanoscale Al–TiN multilayered composites

Nanoscale multilayered Al–TiN composites were deposited using the dc magnetron sputtering technique in two different layer thickness ratios, Al : TiN = 1 : 1 and Al : TiN = 9 : 1. The Al layer thickness varied from 2 nm to 450 nm. The hardness of the samples was tested by nanoindentation using a Berkovich tip. Cross-sectional transmission electron microscopy (TEM) was carried out on samples extracted with focused ion beam from below the nanoindents. The results of the hardness tests on the Al–TiN multilayers with two different thickness ratios are presented, together with observations from the cross-sectional TEM studies of the regions underneath the indents. These studies revealed remarkable strength in the multilayers, as well as some very interesting deformation behavior in the TiN layers at extremely small length scales, where the hard TiN layers undergo co-deformation with the Al layers.     

Comparative study on low energy ion beam modification of thermoplastic polymers

ABSTRACT

Polycarbonate (PC) and polyethylene terephthalate (PET) thermoplastic polymer films were irradiated by low energy ion beams such as 100 keV Hydrogen (H⁺) ions and 350 keV Nitrogen (N⁺) ions at varied fluence from 1?×?10¹³ ions/cm² to 5?×?10¹⁴ ions/cm². The depth profile concentration of ions was calculated using Stopping and Range of Ions in Matter (SRIM) software code. Fourier Transform Infrared (FTIR) technique shows decrement in the intensity of peaks and disappearance of peaks mainly related to carbonyl stretching at 1770?cm^?1 and C–C stretching at 1500?cm^?1. Scanning electron microscopy (SEM) of irradiated polymers showed the formation of pores. X-ray diffraction (XRD) analysis has showed decrease in the intensity indicating the decrease in crystallinity after irradiation. Mechanical studies revealed that the molecular weight and microhardness decrease with increase in ion fluence due to increase in chain scission. The contact angle increased with increase in ion fluence indicating the hydrophobic nature of polymer after irradiation. Antibiofilm activity test of irradiated films shows resistance to Salmonella typhi (S. typhi) pathogen responsible for typhoid. The study shows that Nitrogen ion induces more damage compared to Hydrogen ions and PC films get more modified than PET films.     

Surface ordering near the smectic-A-smectic-C transition in thin, free-standing, liquid-crystal films

Optical reflectivity measurements have been conducted near the smectic-A-smectic-C phase transition in free-standing films with thickness between two and eleven molecular layers. The temperature dependence of the reflectivity in thin film differs significantly from that in thick films. The optical thickness per layer increases in films with two to five layers as a result of cooling, in contrast with thick films. The average layer spacing was found to decrease with decreasing film thickness. Zh. éksp. Teor. Fiz. 111, 949–953 (March 1997) Published in English in the original Russian journal. Reproduced here with stylistic changes by the Translation Editor.     

The ferroelectric and ferromagnetic characterization of CoFe2O4/Pb(Mg1/3Nb2/3)O3-PbTiO3 multilayered thin films

The multiferroic (PMN-PT/CFO)_n (n = 1,2) multilayered thin films have been prepared on SiO₂/Si(1 0 0) substrate with LNO as buffer layer via a rf magnetron sputtering method. The structure and surface morphology of multilayered thin films were determined by X-ray diffraction (XRD) and atom force microscopy (AFM), respectively. The smooth, dense and crack-free surface shows the excellent crystal quality with root-mean-square (RMS) roughness only 2.9 nm, and average grain size of CFO thin films on the surface is about 44 nm. The influence of the thin films thickness size, periodicity n and crystallite orientation on their properties including ferroelectric, ferromagnetic properties in the (PMN-PT/CFO)_n multilayered thin films were investigated. For multilayered thin films with n = 1 and n = 2, the remanent polarization Pr are 17.9 μC/cm² and 9.9 μC/cm²; the coercivity H_c are 1044 Oe and 660 Oe, respectively. In addition, the relative mechanism are also discussed.     

Determination and analysis of the optical constants of thin films of nickel(II) and copper(II) hydrazone complexes by spectroscopic ellipsometry

Thin films of four nickel(II) and copper(II) hydrazone complexes, which will hopefully be used as recording layers for the next-generation of high-density recordable disks, were prepared by using the spin-coating method. Absorption spectra of the thin films on K9 optical glass substrates in the 300–700 nm wavelength region were measured. Optical constants (complex refractive indices N) and thickness d of the thin films prepared on single-crystal silicon substrates in the 275–675 nm wavelength region were investigated on a rotating analyzer-polarizer scanning ellipsometer by fitting the measured ellipsometric angles (Ψ(λ) and Δ(λ)) with a 3-layer model (Si/dye film/air). The dielectric functions ε and absorption coefficients α as a function of the wavelength were then calculated. Additionally, a design to achieve high reflectivity and optimum dye film thickness with an appropriate reflective layer was performed with the Film Wizard software using a multilayered model (PC substrate/reflective layer/dye film/air) at 405 nm wavelength. PACS 81.05.L; 78.20.Ci; 78.20.-e     

Formation of the composition and topography of surface layers of Cu50Ni50 foils under laser irradiation

The influence of the laser radiation power density on the changes in the composition and mechanical properties of surface layers of Cu₅₀Ni₅₀ foils has been investigated using X-ray photoelectron spectroscopy, scanning probe microscopy, X-ray diffraction, and microhardness measurements. It has been found that, after laser irradiation, the redistribution of elements occurs in the surface layer with a thickness of ～30 nm on the irradiated side of the foil. It has been revealed that there are microdistortions in the crystal lattice of the alloy, microdeformations of grains, and variations in the microhardness of the irradiated surface. The mechanisms explaining the observed changes in the foils after laser irradiation have been proposed.     

Crystallization of amorphous SiC and superhardness effect in TiN/SiC nanomultilayers

TiN/SiC nanomultilayers with various constituent layer thicknesses were prepared by magnetron sputtering using TiN and SiC ceramic targets. X-ray diffractometer, scanning electron microscope, energy dispersive spectrometer, high-resolution transmission electron microscope, atomic force microscope and nanoindenter were employed to study the growth, microstructure and mechanical properties of these films. Experimental results revealed that amorphous SiC, which is more favorable under normal sputtering conditions, was forced to crystallize and grew epitaxially with TiN layers at thicknesses of less than 0.8 nm. The resultant films were found to form strong columnar structures, accompanied with a remarkable hardness increment. Maximal nanoindentation hardness as high as 60.6 GPa was achieved when SiC thickness was ∼0.6 nm. A further increase of SiC thickness caused the formation of amorphous SiC, which blocked the epitaxial growth of the multilayers, resulting in the decline of film's hardness. Additionally, investigations on multilayers different in TiN layer thicknesses showed that they are insensitive in both microstructure and hardness to the fluctuation of TiN layer thickness. The formation of epitaxially grown structure between crystalline SiC and TiN layers was found to be responsible for the obtained superhardness in multilayers.     

Influence of the thickness of CdTe and ZnTe layers on cathodoluminescence spectra of strained CdTe/ZnTe superlattices with quantum-dot layers

The influence of the thickness of ZnTe barrier layers on the cathodoluminescence spectra of strained CdTe/ZnTe superlattices containing layers of quantum dots with an average lateral size of approximately 3 nm has been investigated. In samples with thick barrier layers (30, 15 nm), the cathodoluminescence spectra of quantum dots exhibit one band with a maximum at E = 2.03 eV. It has been revealed that, at a barrier layer thickness of ∼3 nm, the luminescence band is split. However, at a ZnTe layer thickness of 1.5 nm, the luminescence spectrum also contains one band. The experimental results have been interpreted with allowance made for the influence of elastic biaxial strains on the energy states of light and heavy holes in the CdTe and ZnTe layers. For the CdTe/ZnTe heterostructure with quantum dots in which the thickness of the deposited CdTe layer is 1.5 monolayers and the thickness of the barrier layer is 100 monolayers, the cathodoluminescence spectrum contains 2LO-phonon replicas. This effect has been explained by the resonance between two-phonon LO states and the difference between the energy states in the electronic spectrum of wetting layer fragments.