In the work, the density of energy states in the valence band of metallic phase nanograins spherical shape with diameters from 1 to 50 nm was calculated. It was found that the energy distances between neighboring energy states in the valence band of metallic phase nanograins are from 0.1 to 2·10-6 eV for the above-mentioned diameter range. There are many orders larger distance, than characteristic for macroscopic-sized metal, the value of which is approximately 10-22 eV. The calculations show that in nanocomposites consisting of metallic phase nanograins with dimensions below 20 nm placed in a dielectric matrix with high resistivity, there is no characteristic for the macroscopic dimensions band conductivity at low temperatures. The results of the calculation of the distance between neighboring energetic states in the valence band of metallic phase nanograins are consistent with the values obtained experimentally.
Nanostructured multicomponent (TiAlSiY)N coatings were fabricated by the vacuum-arc cathodic evaporation (CAPVD). The bias potential was -200 V and -500 V during the deposition process. The nanograin structure with small average crystallite size of about 7.5 nm and [110] preferred orientation were observed in the coatings deposited at high substrate bias (-500 V). Crystallites of about 41.6 nm in size and a preferred orientation with [111] axis were formed in coatings when the bias was -200 V. In this case, the nanostructured coating demonstrated the maximum hardness H = 49.5 GPa (superhardness). Additionally, the studied samples exhibited high abrasion and crack resistance, low wear at tribological tests. The testing of a polycrystalline cubic boron nitride (PCBN) cutter plate covered with (TiAlSiY)N coating fabricated at -200 V revealed an increase in the coefficient of resistance during cutting by 1.66 times in comparison with the base tool material.
The work presents the results of determination of chemical composition of nanocomposites (FeCoZr)x(SiO2)(100-x)produced by ion-beam sputtering in mixed argon-oxygen atmosphere. Atomic percentage of elements of metallic and dielectric phases was obtained for series of composite samples with different metallic phase content x by using of scanning electron microscopy (SEM) with attachment for X-ray microanalysis. Analysis of SEM results showed that ratio of elements forming composition on dielectric phase Y is less then be expected. Electrical properties of nanocomposite (FeCoZr)x(SiO2)(100-x)) were investigated based on measurement of frequencytemperature dependencies of conductivity σ(f, T) and frequency factor α(f, T). The conductivity is almost constant throughout the entire frequency range but increases with increasing temperature for samples with lower metallic phase content x ≤ 55,05 at.%. For samples with x ≥ 61,58 at.% the conductivity have constant values in low-frequency area, then there is an increase in conductivity with further stabilization at higher frequencies. The increase of conductivity on σ(f) corresponds to reaching the maximum values of frequency factor α on the frequency dependencies α(f). The increase in σ along with the increase in frequency indicates an hopping mechanism of conduction of charges in the nanocomposite.
The paper presents temperature-frequency dependencies of conductivity of the granular metal-dielectric nanocomposites (FeCoZr)x(CaF2)100-x. A series of nanocomposite samples with a different metallic phase content from range x = 41.3 – 86.1 at.% produced by twosources ion-beam sputtering in mixed atmosphere of argon and oxygen was tested. Analysis of results of temperature dependences of conductivity of the samples with metallic phase content x bellow 81.8 at.% obtained immediately after producing showed that nanocomposites (FeCoZr)x(CaF2)100-x exhibit dielectric properties, namely conductivity increases with the increase of measurement temperature. At the metal phase content x = 86,1 at.% inverse relationship of conductivity was observed, which menace that nanocomposite is characterized by metallic type of conductivity. Comparison of the conductivity at LNT (liquid nitrogen temperature) and at room temperature for different content of metallic phase allowed to set the percolation threshold for tested series of samples of nanocomposite (FeCoZr)x(CaF2)100-x. The change of type of conductivity from dielectric to metallic type takes place with metallic phase content about 82±0.2at.%.
In this paper the influence of 15-minutes annealing in temperature range 398 K – 723 K with step 25 K on the frequency dependence on conductivity of nanocomposite (FeCoZr)x(CaF2)(100-x) was exanimate. Nanocomposite with metallic phase content x = 81.8 at.% was produced by ion-beam sputtering in mixed argon and oxygen atmosphere. Measurement were made in frequency range 50 Hz – 5 MHz and temperatures from 15 K to 375 K.
It was found that to annealing temperature 523 K in measurement temperatures a less than room temperature a weak dependence of dielectric type of conductivity occurs in materials – the conductivity increases with temperature increase. At temperatures above room temperature a phase transition dielectric-metal is observed and a conductivity decreases with temperature increase. Growth stage of conductivity was observed in the frequency range above 105 Hz. The relaxation time for this stage is of the order 10-6 s. Annealing in the temperature above 523 K led to the appearance of additional low temperature stage of conductivity, for which the relaxation time is of the order of 10-4 s. The appearance of the low-frequency stage of conductivity increase is associated with oxidation of surface of nanoparticles of metallic phase during annealing, the growing barrier of potential and relaxation time. Further increase of annealing temperature above 673 K causes a further increase of the width of the barrier, and activation energy becomes so much that relaxation times for low-frequency stage grown above 10-2 s. Therefore, low-frequency stage is moves further into the area of low frequency and it becomes unnoticeable because it go beyond the lower range (50 Hz) of used meter.
In this work thermogravimetric-DTG/DSC analysis result for samples of nanocomposite metal-dielectric (FeCoZr)x(CaF2)100-x are presents. Series of samples with, metallic phase content x = 24 – 68 at.% were produced by ionbeam sputtering method in mixed atmosphere of gas argon and oxygen. Study of thermal properties, phase shifts and process of change in mass of nanocomposites were performed using the thermoanalytical system TGA/DSC-1/1600 HF (MettlerToledoInstruments). High-precision weight has a weighing range 1μg – 1g with an accuracy 1μg. The furnace makes it possible to regulate the temperature in range from room temperature to 1600°С and heating rate is 0.01 – 150°С/min. After analysis of the results established that initial and final mass of samples of the nanocomposite (FeCoZr)x(CaF2)100-x are different, namely the sample mass is increased by 2 – 20%. It is related to the oxidation of metallic phase particles of nanocomposite. DTG and DSC analysis demonstrated that oxidation of metallic phase is held in two steps, at first oxidized iron atoms, and followed oxidation of the cobalt atoms, what can be seen on the waveform in the form of two humps and whereby oxides Fe2O3, Fe3O4, Co2O3, Co3O4 are formed. Oxide coatings on the surface of atoms represents an additional barrier to electron transfer charges. When a voltage is applied to the layer of the nanocomposite are three possible ways to transfer of charges between atoms and particles of metal, whereby each has its own relaxation time.
In this work, the temperature and frequency dependences of conductivity σ and Arrhenius plots of annealed nanocomposite films containing Fe45Co45Zr10 - based nanoparticles embedded in a doped PbZrTiO3 ferroelectric matrix were studied. The nanocomposites studied were deposited by sputtering with use of argon and oxygen ions in a vacuum chamber. Tested samples were followed by a 15-min annealing process in air in the temperature range of 398 K ≤ Ta ≤ 748 K with steps of 25 K. The σ(f,T) dependences of nanocomposite samples was measured in ambient temperature range of 77 K < Tp < 373 K at frequencies of 50 Hz < f < 1MHz. It was established that nanocomposite sample with metallic phase content x = 55.6 at.% demonstrates strong temperature and frequency dependences, which is typical for a percolation systems. Type of conduction in such nanostructure is defined as dielectric, which may be related with the additional oxidation of metallic nanoparticles during the annealing process. For the tested sample with x = 88.4 at.%. we observe metallic type of conduction, when metallic nanoparticles form a permanent conductive channels in dielectric matrix.
The paper presents frequency f and temperature Tp dependences of conductivity σ, capacitance Cp and phase shift angle θ for the nanocomposite metal-dielectric (FeCoZr)x(CaF2)(100-x). Samples of nanocomposite were produced by ion-beam sputtering in pure argon Ar atmosphere. Partial pressure of gas Ar in the ion source pAr=1.1·10-1Pa. Contains of metallic phase in tested sample is x = 54.6 at.%. Studies carried out by stand to measuring of AC electrical properties of nanocomposites and semiconductors. The measurements have been performed using alternating current within the frequency range of 50 Hz - 1 MHz for measuring temperatures ranging from 77 K to 373 K. On the frequency-temperature dependence of phase shift angle θ at low frequencies phase shift have capacitive character and at high frequencies - inductive. Position of fmin on the frequency dependence on capacitance Cp corresponds exactly to the resonance frequency fR for which the angle θ crosses zero. Analysis of the results showed that phenomena similar to phenomena in conventional circuit RLC occur in the nanocomposite (CoFeZr)54.6(CaF2)45.4. Jumping recharging between the defects leads to the formation of dipoles and consequently to the increase of permittivity. After a time τ electron returns to the first defect and dipole disappears. The formation of inductance in nanocomposite is associated with return jumps of electrons from defect with negative charge to the defect with positive charge, set by the time, which are characterized by low values of activation energy.
In this paper results of researches of electrical properties of nanocomposites, in which metallic phase is diamagnetic copper in dielectric SiO2 matrix. Materials were obtained by ion-beam sputtering in argon atmosphere. Measured parameters were resistance Rp, capacity Cp and phase angle θ on AC in frequency range 50 Hz - 5 MHz and in measurement temperature function from the range 77 K - 373 K. Based on obtained results occurrence of positive values of phase angle was established. These values were observed in materials immediately after preparation and in annealed in temperature 398 K. Occurrence of non-coil inductance and in some cases voltage resonance phenomena were determined.
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