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This paper demonstrates the influence of deposition parameters (temperature, power and time) and stoichiometric composition of thin aluminum nitride (AlN) coatings, the thickness of which varied from 320 to 1100nm deposited by DC reactive magnetron sputtering on their microstructure, mechanical and microtribological properties. The investigation revealed that high-deposition power (150W) and temperature (200∘C) lead to sputtering of coatings with high roughness, low mechanical and high microtribological properties. Such a phenomenon occurred due to the formation of a coarse-grained structure, high porosity and dendritic growth of the coating, which was observed on their cross-sections. Reducing the deposition temperature to 20∘C and power to 80–100W allowed to obtain a fine-crystalline structure demonstrating low-roughness values with crystallites evenly and compactly distributed over the surface. Such coatings showed higher mechanical and low microtribological properties. Surface resistivity was lower on coatings with a fine crystalline structure and correlated with the nitrogen content of the coating. In the course of the research, it was demonstrated that the optimal combination of microstructure, mechanical, microtribological properties and electrical resistivity for practical use in micro- and nanosensory applications may be achieved for the AlN coating with the thickness of 320nm and 29.71at.% N, deposited at 20∘C, 100W and 20min. Such a coating possesses the highest values of mechanical properties, low roughness and specific surface resistance, as well as low coefficient of friction and specific volumetric wear compared to all coatings under study.
Bulk metallic glasses synthesized at specialized facilities at Yale using magnetron cosputtering are sent to Southern Connecticut State University for elemental characterization. Characterization is done using a Zeiss Sigma VP SEM coupled with an Oxford EDS. Characterization is automated using control software provided by Oxford. Collected data is processed and visualized using computational methods developed internally. Processed data is then organized into a database suitable for web retrieval. This technique allows for the rapid characterization of a combinatorial wafer to be carried out in ~11 hours for a single wafer containing ~600 unique compounds.
Aluminium nitride (AlN) thin films were fabricated on a glass substrate by reactive magnetron sputtering. Raman microscopy was then employed to follow the characteristics of their optical and acoustic phonon modes. At the optimal sputtering time of 30 minutes, the defect-induced first and second order Raman spectra were observed in 400–800 cm-1 band which were mostly related to the coating compositions. However, at the 30-, 60- and 90-minute sputtering, crystals of submicron size order of AlN were achieved. This could be clearly identified by the presence of Raman peak at 658–662 cm-1. Powder X-ray diffraction (PXRD) patterns revealed the development of (002) and (101) planes of hexagonal wurtzite AlN phase. The optimal average grain size measured by atomic force microscopy (AFM) is at 330 nm. It was found that the hardness was strongly dependent on roughness of the film, the maximum of which was achieved at 20.00 GPa. The presence of F-type defects in AlN films was investigated by X-band (~9.44 GHz) ESR spectrometer at 295 K. The ESR experiments were carried out by applying magnetic field perpendicular to AlN film, which showed the ESR six-peak multiplet signal at ~290 mT arising from superhyperfine interactions between nuclear spin I = 5/2 of 27Al and electron spins trapped in nitrogen vacancies. The ESR signals are simulated and the ESR parameters are calculated. The vacancies are clearly randomly distributed as the ESR signals are independent of rotation angle (φ) about the normal of the film. All these results were analyzed and presented as a function of the deposition parameters and composition, and crystalline phases existed in the films.
SiCN nanoparticle films were prepared by plasma RF magnetron sputtering under a mixture flow of N2, Ar, and H2, and optimized in visible photoluminescence (PL) by controlling the N2 flux. The highest PL intensity was obtained as the N2 flow rate was set at a moderate value, i.e. 6.4 sccm when the flow rates of Ar and H2 were 35.2 and 9.6 sccm, respectively. Furthermore, for the sample grown at 400°C, a significant improvement in photoluminescence can be achieved with annealing at 1100°C under N2 protection, in contrast to that grown at room temperature. The structure and chemical bonding analyzed by X-ray diffraction, X-ray photoelectron spectrum, and Fourier-Transform Infrared spectrum, respectively, revealed that the content of the SiCN nanoparticle, C–N, N–H, and Si–O bonds significantly affect the PL in theSiCN nanoparticle films.
By controlling the sputtering power, rotated speed of substrate and sputtering time, Ni–Cr films with appropriate composition were fabricated by double-target magnetron co-sputtering techniques. The cross-sectional micrograph and element diffusion of Ni–Cr films deposited on stainless steel substrates by magnetron sputtering have been analyzed by scanning electron microscope (SEM) and energy dispersive spectroscope (EDS). The results indicate that the according compositions of Ni–Cr films are 58 wt.% Ni and 42 wt.% Cr when the sputtering powers of Ni and Cr targets are 288 W and 280 W, respectively. In the same time, the diffusions of Ni, Fe and Cr were revealed and the diffusion distances of Ni and Cr are calculated by Fick's second law with a Pile-Up law model. The largest diffusion distance is about 885 nm, beyond which the content of Ni and Cr detected by EDS is the same as the substrate.
The electromechanical properties of nichrome (Ni–Cr 80/20 wt.%) used as a common material for application in thin film strain gauges have been studied. The surface topography and chemical composition of Ni–Cr thin films grown on the glass substrate by magnetron sputtering have been analyzed by atomic force microscope (AFM) and energy dispersive spectroscopy (EDS), respectively. The temperature coefficient of resistance (TCR) has been determined by a Nano-volt/Micro ohm meter. The gauge factor (FG) has been determined by the cantilever method. Low stable TCR values (22 ppm to 46 ppm in the 50–150°C temperature range) have been obtained. Resistance stability is achieved by rapid thermal annealing (RTA) at 300°C for 10 min combined with a 24 h thermal annealing (TA) at 150°C. The desired 45 Ω/m sheet resistance and a gauge factor of 2.6 have been attained for 40-nm-thickness films. The films have very small roughness of 2.1~4.4 nm.
By controlling the sputtering power, rotational speed of the substrate and sputtering time, Ni–Cr thin films with appropriate composition were fabricated by double-target magnetron co-sputtering techniques. The homogeneity and oxidation of Ni–Cr thin film has been studied by Auger electron spectroscopy (AES). The structures of Ni–Cr thin films were determined by an X-ray diffractometer (XRD). The oxidation and the resistance stability of the Ni–Cr thin film after rapid thermal process (RTP) have been studied. The relations between TCR and RTP techniques of Ni–Cr thin films were discussed.
Molybdenum nitride films γ-Mo2N/Si have been fabricated with reactive magnetron sputtering in (N2 + Ar) gas mixture. Phase composition of the films has been defined with reflection high energy electron diffraction. Refractive index and extinction coefficient of γ-Mo2N have been evaluated with laser ellipsometry at λ = 632.8 and 488.0 nm. Upper limit of γ-Mo2N film thickness measurable with laser ellipsometry has been found to be ~80 nm.
In-doped zinc oxide (ZnO:In) thin films with thickness from 157 nm to 592 nm have been deposited on glass substrates by radio frequency (RF) magnetron sputtering. The effect of the film thickness on the structural, electrical and optical properties of ZnO:In thin films has been investigated. It is found that the films are hexagonal wurtzite structure with c-axis perpendicular to the substrate, and with increasing thickness, the crystallinity, the grains size and the conductivity of the films increases, but the strains along c-axis and the transmittance decrease. The decrease of the resistivity in a thicker film is attributed to the slight increase of the carrier concentration and the significant increase of Hall mobility. The transmittance of all the films is over 80% in the visible region (400–800 nm) and the band gap decrease with the increase of film thickness. The film with the thickness of around 303 nm has the resistivity of 6.07 × 10-3 Ω⋅cm and the transmittance of 90% in the visible range. Based on the good conductivity and high transmittance, the ZnO:In films prepared by magnetron sputtering can be regarded as a potential transparent electrode.
Sm-doped BaTiO3 thin films with ~200 nm thickness fabricated by rf magnetron sputtering system onto Pt/Ti/SiO2/Si substrates have been investigated. The effects of postannealing and the dopant content in a range of 0.1 to 2.2 at.% on microstructure and electrical properties were studied. The films were found to be amorphous in the as-deposited state and became fully crystallized after annealing at 750°C and above. The addition of Sm in the BaTiO3 films resulted in the inhibition of grain growth. Electrical characterizations show that the dielectric permittivity increased with increasing annealing temperatures and the 2.2% Sm-doped film had the low leakage current of 1.29×10-9 A at an applied electric field of 100 KV/cm.
Submicron zinc oxide (ZnO) spheres prepared by a two-stage hydrothermal method were assembled into a layer on a substrate by vertical deposition. Vanadium pentoxide (V2O5) was deposited onto the top of ZnO spheres by magnetron sputtering followed by annealing in oxygen atmosphere at 500∘C for an hour. The microstructures and optical properties of the prepared samples were investigated. The photoluminescence (PL) results indicate that the intensity of PL in the annealed ZnO/V2O5 composite microstructures is dramatically improved compared to the constituent V2O5 and ZnO spheres. The intensity enhancement of light emission from the ZnO/V2O5 composite may be attributed to the special microstructure of ZnO particles and the coupling effect between ZnO and V2O5. This transition oxide composite may possibly be developed into a new type of high-efficiency light emitting material.
Growth of Sb/SiNx multilayers, followed by high-temperature annealing, was shown to be an effective strategy for synthesizing Sb-doped Si quantum dots (Si-QDs). The doping concentration of Sb (from 0.32 at.% to 1.82 at.%) was controlled by varying the thickness of Sb sublayer. Moderate Sb concentrations were found to enhance the formation of Si-QDs. Photoluminescence (PL) results show that the nonradiative recombination defects caused by Sb impurities increased with the increase of Sb content, which leads to the decrease of the emission intensity. Hall measurements demonstrate that as the carrier concentration increases, the mobility of Hall decreases, and the conductivity increases at first and then decreases with the increase of Sb content. It is indicated that the excessive high Sb doping will deteriorate the conductive properties. The observed n-type electrical behavior and great enhancement increase in conductivity of the Sb-doped Si-QDs film suggest an effective Sb doping. A p–n junction was formed between Sb-doped Si-QDs and a p-type c-Si substrate, exhibiting good rectifying properties.
Thin films of topological insulator (TI) Bi2Se3 were grown onto the surfaces of FeSe2 layers of different thicknesses on Si (100) substrates by magnetron sputtering, forming bilayer films with smooth surface. Magnetic and transport measurements indicate ferromagnetism in these bilayer samples. Large coercive fields at low-temperatures and a room-temperature magnetic order were observed. Moreover, nonsaturated high-filed linear magnetoresistance (MR) and weak anti-localization effect were found in these bilayer thin films. These results indicate that the bilayer samples could have both strong spin–orbit coupling and ferromagnetic proximity effect, which are the desired features.
Chromium-carbon films have been deposited on silicon substrates by magnetron sputtering of chromium and carbon targets in pure argon atmosphere. The composition of the films was examined by Auger electron spectroscopy. Oxygen, nitrogen, and iron were the major impurities incorporated in the films. The mechanical and electrical properties of the films were investigated as a function of negative bias voltage applied to substrates. The hardness and elastic modulus were measured by a nano-indenter and the values are around 17.0±0.9 GPa and 245±11 GPa, respectively. The hardness and elastic modulus of the films increased while the electrical resistivity decreased when the substrate bias voltage was applied. The lowest resistivity (~ 267 μohm-cm) was obtained at the substrate bias voltage of 50 V. The temperature dependence of resistivity of the films was measured in air from room temperature to 673 K. The time dependence of resistivity of the films was also measured in air at 673 K. It was found that the resistivity changed little with temperature or time.
A series of nitrogen-doped Zn0.93Co0.07O thin films grown on glass substrates were prepared by magnetron sputtering, which have shown ferromagnetic property at room temperature. The largest moment of about 4.92 μB/Co and Curie temperature (Tc) of about 300 K were observed for Zn0.93Co0.07O thin film. P-type Co-doped ZnO thin films with room temperature ferromagnetism were obtained. We demonstrated a clear correlation between nitrogen and transition temperature and an inverse correlation between nitrogen and magnetization per Co ion.
TaN thin films were deposited on Al2O3 wafers by DC reactive magnetron sputtering. The composition control by nitrogen partial flux in the working gas and the electrical properties of the samples were investigated in detail. The results show that the atomic number ratio of Ta to N in the samples can be adjusted from 4 to 0.88, corresponding to the contents of N in the samples from 20 at.% to 53 at.%, by adjusting the nitrogen partial flux from 2% to 6%. The main phases in the TaNx thin films are hexagonal Ta2N, body centered cubic Ta10N and face centered cubic TaN at lower N contents (lower than 28 at.%). However, at higher N contents (higher than 28 at.%), orthorhombic Ta3N5 phase gradually precipitates out from the samples, and the hexagonal Ta2N phase disappears. When the N contents in the samples are lower than 28 at.%, the sheet resistance and resistivity of TaNx thin films are all low. With further increase of the N contents, the sheet resistance and resistivity of TaNx thin films increase sharply. The sheet resistance and the resistivity of the samples can be adjusted from 17 Ω/sq. to 77 Ω/sq., from 344 μΩ ·cm to 1030 μΩ ·cm by adjusting the nitrogen contents, respectively. When the nitrogen contents in the samples are lower than 28 at.%, the TCR of the samples is less than 50 ppm/°C. With further increase of N contents, the TCR of the samples increases sharply up to a few hundred ppm/°C.
CdTe-doped SiO2 thin films were produced by RF magnetron co-sputtering technique. Presence of CdTe nanocrystals inside the silica matrix was confirmed by Raman spectroscopy and grazing incidence X-ray diffraction. The samples demonstrate size dependent photoluminescence. Temperature dependent photoluminescence measurements were carried out in the temperature range 15–295 K and revealed energy-emission thermal stability. This feature can be usefully applied in a production of light-emitting diodes with wavelength stability in a wide temperature range.
10-nm-thick amorphous LaAlO3 film was deposited on n-type Si (001) substrate at 600°C by magnetron sputtering and then annealed in N2 ambience at 300°C for 2 min using a rapid thermal annealing furnace. Grazing incidence X-ray diffraction analyses indicated that the post-annealed LaAlO3 film was still amorphous. The root-mean-square roughness of the post-annealed sample is a little smaller than that of the as-grown sample, which could stem from the densification of LaAlO3 film after post-annealing. No obvious hysteretic behavior was observed in the capacitance–voltage measurement and the dielectric constant of LaAlO3 film was estimated to be 16.7. Due to the deficiency of oxygen vacancy after post-annealing, the low leakage current density of the post-annealed film with EOT of 2.33 nm is about 5.52 × 10-5 A/cm2 at +1 MV/cm. Moreover, it is found that both the as-grown and post-annealed capacitors satisfy Ohmic conduction behavior at the whole positive measured electric fields.
Amorphous V2O5, LiPON and Li2Mn2O4 thin films were fabricated by RF magnetron sputtering methods and the morphology of thin films were characterized by scanning electron microscopy. Then with these three materials deposited as the anode, solid electrolyte, cathode, and vanadium as current collector, a rocking-chair type of all-solid-state thin-film-type Lithium-ion rechargeable battery was prepared by using the same sputtering parameters on stainless steel substrates. Electrochemical studies show that the thin film battery has a good charge–discharge characteristic in the voltage range of 0.3–3.5 V, and after 30 cycles the cell performance turned to become stabilized with the charge capacity of 9 μAh/cm2, and capacity loss of single-cycle of about 0.2%. At the same time, due to electronic conductivity of the electrolyte film, self-discharge may exist, resulting in approximately 96.6% Coulombic efficiency.
The stacked precursors were deposited on glass substrates from Cu, Sn and ZnS targets by magnetron sputtering with six kinds of stacking sequences. The precursors were sulfurized at 500°C for 2 h in an atmosphere of sulfur. The properties of thin films such as microstructure, morphology, chemical composition, electrical and optical properties of the films were investigated by X-ray diffraction (XRD), scanning election microscopy (SEM), energy dispersive spectroscopy (EDS), Hall effect measurements and UV-visible spectrophotometer (UV-VIS). The results show that the thin film after sulfurizing at 500°C using the stacking order of Cu/Sn/ZnS/glass is the best absorber layer for Cu2ZnSnS4 thin films solar cell among the six kinds of stacking sequences.