Analysis of Structural and Photocatalytical Properties of Anatase, Rutile and Mixed Phase TiO2 Films Deposited by Pulsed-Direct Current and Radio Frequency Magnetron Co-Sputtering

Amongst many water purification techniques, TiO2 photocatalysis is recognized as one of the most promising sustainable methods. It is known that for photocatalytical applications anatase is the most suitable TiO2 phase, however heterojunction of anatase/rutile phases could improve the photocatalytical activity of TiO2 even further. Despite the relative simplicity of TiO2 different synthesis methods lead to the highly dispersed crystal phases and photocatalytic activity of the corresponding samples. Accordingly, suggestions and investigations of various innovative methods of TiO2 synthesis are still needed. In this work structural and photocatalytical properties of TiO2 films deposited by the unconventional method of simultaneous co-sputtering from two magnetrons powered by pulsed-Direct Current (pDC) and Radio Frequency (RF) power sources with negative bias voltage have been studied. More specifically, TiO2 film thickness, microstructure, surface roughness, crystal structure, optical transmittance and photocatalytical properties were investigated by profilometer, scanning electron microscope, atomic force microscope, X-ray diffractometer and UV-Vis spectrophotometer respectively. The proposed unconventional two magnetron co-sputtering based TiO2 film formation method showed very promising results for crystalline TiO2 film formation while keeping process temperatures below 100 °C. XRD analysis revealed that by using proper combination of power source type and bias voltage various TiO2 phases (amorphous, anatase, rutile or their mixture) can be synthesized selectively. Moreover, strong dependency between power source type and surface roughness, as well as between the bias voltage and band gap value of TiO2 films was observed. Interestingly, TiO2 films deposited by two magnetron co-sputtering without bias voltage had one of the highest band gap values between the investigated films but its photocatalytic activity was superior compared to all other samples. It is suggested that this is due to the dominating nanocrystalline anatase phase with various exposed surfaces including photocatalytically the most active {001}.

Studies on the Characterization and Machinability of Duplex Stainless Steel 2205 during Dry Turning

The present investigation is a study of the effect of advanced Physical Vapor Deposition (PVD) coatings on cutting temperature residual stresses and surface roughness during Duplex Stainless Steel (DSS) 2205 turning. Austenite stabilizers like nickel, manganese, and molybdenum reduced the cost of DSS. Surface Integrity (SI) plays an important role in determining corrosion resistance and fatigue life. Resistance to various types of corrosion makes DSS suitable for applications with critical environments like Heat exchangers, Desalination plants, Seawater pipes and Marine components. However, lower thermal conductivity, poor chip control and non-uniform tool wear make DSS very difficult to machine. Cemented carbide tools (M grade) were used to turn DSS in a dry environment. AlTiN and AlTiCrN coatings were deposited using advanced PVD High Pulse Impulse Magnetron Sputtering (HiPIMS) technique. Experiments were conducted with cutting speed of 100 m/min, 140 m/min and 180 m/min. A constant feed and depth of cut of 0.18 mm/rev and 0.8 mm were used, respectively. AlTiCrN coated tools followed by AlTiN coated tools outperformed uncoated tools due to properties like lower thermal conductivity, higher adhesion strength and hardness. Residual stresses were found to be compressive for all the tools used for dry turning, increasing the fatigue life of the machined component. Higher cutting temperatures were observed for coated tools due to its lower thermal conductivity, which results in very less tool wear than uncoated tools. Surface roughness with uncoated tools was found to be three times higher than coated tools due to lower coefficient of friction of coating used.

Fabrication and Characterization of Al2O3 Based Electrical Insulation Coatings Around SiC Fibers

In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al2O3)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al2O3 respectively. Raman spectroscopic analyses produced no characteristic bands of Al2O3, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Influence of Argon Gas Concentration in N2-Ar Plasma for the Nitridation of Si in Abnormal Glow Discharge

Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si3N4 confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N2 plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Unbalanced Cylindrical Magnetron for Accelerating Cavities Coating

We report in this paper the design and qualification of a cylindrical unbalanced magnetron source. The dedicated magnetic assemblies were simulated using a finite element model. A hall-effect magnetic probe was then used to characterize those assemblies and compared to the theoretical magnetic profiles. These show a good agreement between the expected and actual values. The qualification of the different magnetic assemblies was then performed by measuring the ion flux density reaching the surface of the sample to be coated using a commercial retarding field energy analyzer. The strongest unbalanced configuration shows an increase from 0.016 A.cm-2 to 0.074 A.cm-2 of the ion flux density reaching the sample surface compared to the standard balanced configuration for a pressure 5.10-3 mbar and a plasma source power of 300 W.

The Effect of the Deposition Parameters on the Microstructural and Optical Properties of Mn-Doped GeTe Chalcogenide Materials

In this work, the effect of the magnetron sputtering system parameters on the optical properties of the Mn doped GeTe were investigated. The optical properties of the Ge1-xMnxTe thin films with different thicknesses are determined by analyzing the transmittance and reflectance data. The energy band gaps of the amorphous Mn-doped GeTe thin films with different thicknesses were calculated. The obtained results demonstrated that the energy band gap values of the amorphous films are quite different and they are dependent on the films thicknesses. The extinction coefficients of amorphous Mn-doped GeTe thin films as function of wavelength for different thicknesses were measured. The results showed that the extinction coefficients of all films are varying inversely with their optical transmission. Moreover, the results emphasis that, not only the microstructure, electrical and magnetic properties of Mn doped GeTe thin films vary with the films thicknesses but also the optical properties differ with the film thickness.

Response Surface Methodology for Optimum Hardness of TiN on Steel Substrate

Hard coatings are widely used in cutting and forming tool industries. Titanium Nitride (TiN) possesses good hardness, strength, and corrosion resistance. The coating properties are influenced by many process parameters. The coatings were deposited on steel substrate by changing the process parameters such as substrate temperature, nitrogen flow rate and target power in a D.C planer magnetron sputtering. The structure of coatings were analysed using XRD. The hardness of coatings was found using Micro hardness tester. From the experimental data, a regression model was developed and the optimum response was determined using Response Surface Methodology (RSM).

Mechanical Properties and Microstructural Properties of CrSiN Coating

The present study deals with the characterization of CrSiN coatings obtained by PVD magnetron sputtering systems. CrSiN films were deposited with different Si contents, in order to check the effect of at.% variation on the different properties of the Cr–N system. Coatings were characterized by scanning electron microscopy (SEM) for thickness measurements, X-ray diffraction. Surface morphology and the roughness characteristics were explored using AFM, Mechanicals properties, elastic and plastic deformation resistance of thin films were investigated using nanoindentation test. We observed that the Si addition improved the hardness and the Young’s modulus of the Cr–N system. Indeed, the hardness value is 18,56 GPa for CrSiN coatings. Besides, the Young’s modulus value is 224,22 GPa for CrSiN coatings for Si content of 1.2 at.%.

The Effect of Aging of ZnO, AZO, and GZO Films on the Microstructure and Photoelectric Property

RF magnetron sputtering is used on the ceramic targets, each of which contains zinc oxide (ZnO), zinc oxide doped with aluminum (AZO) and zinc oxide doped with gallium (GZO). The XRD analysis showed a preferred orientation along the (002) plane for ZnO, AZO, and GZO films. The AZO film had the best electrical properties; it had the lowest resistivity of 6.6 × 10-4 cm, the best sheet resistance of 2.2 × 10-1 Ω/square, and the highest carrier concentration of 4.3 × 1020 cm-3, as compared to the ZnO and GZO films.

Nanoindentation of Thin Films Prepared by Physical Vapor Deposition

These Monolayer and multilayer coatings of CrN and AlCrN deposited on 100Cr6 (AISI 52100) substrate by PVD magnetron sputtering system. The microstructures of the coatings were characterized using atomic force microscopy (AFM). The AFM analysis revealed the presence of domes and craters that are uniformly distributed over all surfaces of the various layers. Nanoindentation measurement of CrN coating showed maximum hardness (H) and modulus (E) of 14 GPa and 190 GPa, respectively. The measured H and E values of AlCrN coatings were found to be 30 GPa and 382 GPa, respectively. The improved hardness in both the coatings was attributed mainly to a reduction in crystallite size and decrease in surface roughness. The incorporation of Al into the CrN coatings has improved both hardness and Young’s modulus.

Deposition of Transparent IGZO Conducting Thin Films by Co-Sputtering of Zn2Ga2O3 and In2O3 Targets at Room Temperature

In this study, we investigated (In,Ga,Zn)Ox (IGZO) thin films and examined their characteristics of using Ga2O3-2 ZnO (GZO) co-sputtered In2O3 prepared by dual target radio frequency magnetron sputtering at room temperature in a pure Ar atmosphere. RF powers of 80 W and 70 W were used for GZO and pure In2O3, room temperature (RT) was used as deposition temperature, and the deposition time was changed from 15 min to 60 min. Structural, surface, electrical, and optical properties of IGZO thin films were investigated as a function of deposition time. Furthermore, the GZO co-sputtered In2O3 thin films showed a very smooth and featureless surface and an amorphous structure regardless of the deposition time due to the room temperature sputtering process. We would show that the co-sputtered IGZO thin films exhibited transparent electrode properties with high transmittance ratio and low resistivity.

The Microstructure of Aging ZnO, AZO, and GZO Films

RF magnetron sputtering is used on the ceramic targets, each of which contains zinc oxide (ZnO), zinc oxide doped with aluminum (AZO) and zinc oxide doped with gallium (GZO). The electric conduction mechanism of the AZO and GZO films came mainly from the Al and Ga, the oxygen vacancies, Zn interstitial atoms, and Al and/or Ga interstitial atoms. AZO and GZO films achieved higher conduction than did ZnO film, it being ion vacant and nonstoichiometric. The XRD analysis showed a preferred orientation along the (002) plane for ZnO, AZO, and GZO films.

Design and Fabrication of an Electrostatically Actuated Parallel-Plate Mirror by 3D-Printer

In this paper, design and fabrication of an actuated parallel-plate mirror based on a 3D-printer is described. The mirror and electrode layers are fabricated separately and assembled thereafter. The alignment is performed by dowel pin-hole pairs fabricated on the respective layers. The electrodes are formed on the surface of the electrode layer by Au ion sputtering using a suitable mask, which is also fabricated by a 3D-printer.For grounding the mirror layer, except the contact area with the electrode paths, all the surface is Au ion sputtered. 3D-printers are widely used for creating 3D models or mock-ups. The authors have recently proposed that these models can perform electromechanical functions such as actuators by suitably masking them followed by metallization process. Since the smallest possible fabrication size is in the order of sub-millimeters, these electromechanical devices are named by the authors as SMEMS (Sub-Milli Electro-Mechanical Systems) devices. The proposed mirror described in this paper which consists of parallel-plate electrostatic actuators is also one type of SMEMS devices. In addition, SMEMS is totally environment-clean compared to MEMS (Micro Electro-Mechanical Systems) fabrication processes because any hazardous chemicals or gases are utilized.

Production of Size-Selected Tin Nanoclusters for Device Applications

This work reports on the fabrication of tin nanoclusters by sputtering and inert-gas condensation inside an ultra-high vacuum compatible system. This technique allows to fine tune the size and yield of nanoclusters by controlling the nanocluster source parameters. The produced nanoclusters are deposited on SiO2/Si substrate with pre-formed electrical electrodes to produce a nanocluster device. Those devices can be potentially used for gas sensor applications.

In vitro and in vivo Anticancer Activity of Nanosize Zinc Oxide Composites of Doxorubicin

The nanotechnology offers some exciting possibilities in cancer treatment, including the possibility of destroying tumors with minimal damage to healthy tissue and organs by targeted drug delivery systems. Considerable achievements in investigations aimed at the use of ZnO nanoparticles and nanocontainers in diagnostics and antitumor therapy were described. However, there are substantial obstacles to the purposes to be achieved by the use of zinc oxide nanosize materials in antitumor therapy. Among the serious problems are the techniques of obtaining ZnO nanosize materials. The article presents a new vector delivery system for the known antitumor drug, doxorubicin in the form of polymeric (PEO, starch-NaCMC) hydrogels, in which nanosize ZnO film of a certain thickness are deposited directly on the drug surface on glass substrate by DC-magnetron sputtering of a zinc target. Anticancer activity in vitro and in vivo of those nanosize zinc oxide composites is shown.

New Drug Delivery System for Cancer Therapy

The paper presents a new drugs delivery system, based on the thin film technology. As a model antitumor drug, highly toxic doxorubicin is chosen. The system is based on the technology of obtaining zinc oxide composite of doxorubicin by deposition of nanosize ZnO films on the surface of doxorubicin coating on glass substrate using DC magnetron sputtering of zinc targets in Ar:O2 medium at room temperature. For doxorubicin zinc oxide compositions in the form of coatings and gels with 180-200nm thick ZnO films, higher (by a factor 2) in vivo (ascitic Ehrlich's carcinoma) antitumor activity is observed at low doses of doxorubicin in comparison with that of the initial preparation at therapeutic doses. The vector character of the doxorubicin zinc oxide composite transport to tumor tissues ensures the increase in antitumor activity as well as decrease of toxicity in comparison with the initial drug.

Composition Dependent Formation of Sputtered Co-Cu Film on Cr Under-Layer

Sputtered CoxCu100-x films with the different compositions of x = 57.7, 45.8, 25.5, 13.8, 8.8, 7.5 and 1.8 were deposited on Cr under-layer by RF-sputtering. SEM result reveals that the averaged thickness of Co-Cu film and Cr under-layer are 92 nm and 22nm, respectively. All Co-Cu films are composed of Co (FCC) and Cu (FCC) phases in (111) directions on BCC-Cr (110) under-layers. Magnetic properties, surface roughness and morphology of Co-Cu films are dependent on the film composition. The maximum and minimum surface roughness of 3.24 and 1.16nm are observed on the Co7.5Cu92.5 and Co45.8Cu54.2films, respectively. It can be described that the variance of surface roughness of the film because of the difference of the agglomeration rate of Co and Cu atoms on Cr under-layer. The Co57.5Cu42.3, Co45.8Cu54.2 and Co25.5Cu74.5 films shows the ferromagnetic phase whereas the rest of the film exhibits the paramagnetic phase at room temperature. The saturation magnetization, remnant magnetization and coercive field of Co-Cu films on Cr under-layer are slightly increased with increasing the Co composition. It can be concluded that the required magnetic properties and surface roughness of the Co-Cu film can be adapted by the adjustment of the film composition.

Flexible Sensor Array with Programmable Measurement System

This study is concerned with pH solution detection using 2 × 4 flexible sensor array based on a plastic polyethylene terephthalate (PET) substrate that is coated a conductive layer and a ruthenium dioxide (RuO2) sensitive membrane with the technologies of screen-printing and RF sputtering. For data analysis, we also prepared a dynamic measurement system for acquiring the response voltage and analyzing the characteristics of the working electrodes (WEs), such as sensitivity and linearity. In this condition, an array measurement system was designed to acquire the original signal from sensor array, and it is based on the method of digital signal processing (DSP). The DSP modifies the unstable acquisition data to a direct current (DC) output using the technique of digital filter. Hence, this sensor array can obtain a satisfactory yield, 62.5%, through the design measurement and analysis system in our laboratory.

Long-term Monitor of Seawater by using TiO2:Ru Sensing Electrode for Hard Clam Cultivation

The hard clam (meretrix lusoria) cultivated industry has been developed vigorously for recent years in Taiwan, and seawater quality determines the cultivated environment. The pH concentration variation affects survival rate of meretrix lusoria immediately. In order to monitor seawater quality, solid-state sensing electrode of ruthenium-doped titanium dioxide (TiO2:Ru) is developed to measure hydrogen ion concentration in different cultivated solutions. Because the TiO2:Ru sensing electrode has high chemical stability and superior sensing characteristics, thus it is applied as a pH sensor. Response voltages of TiO2:Ru sensing electrode are readout by instrument amplifier in different sample solutions. Mean sensitivity and linearity of TiO2:Ru sensing electrode are 55.20 mV/pH and 0.999 from pH1 to pH13, respectively. We expect that the TiO2:Ru sensing electrode can be applied to real environment measurement, therefore we collect two sample solutions by different meretrix lusoria cultivated ponds in the Yunlin, Taiwan. The two sample solutions are both measured for 200 seconds after calibration of standard pH buffer solutions (pH7, pH8 and pH 9). Mean response voltages of sample 1 and sample 2 are -178.758 mV (Standard deviation=0.427 mV) and -180.206 mV (Standard deviation =0.399 mV), respectively. Response voltages of the two sample solutions are between pH 8 and pH 9 which conform to weak alkali range and suitable meretrix lusoria growth. For long-term monitoring, drift of cultivated solutions (sample 1 and sample 2) are 1.16 mV/hour and 1.03 mV/hour, respectively.

Interfacial Layer Effect on Novel p-Ni1-xO:Li/n-Si Heterojunction Solar Cells

This study fabricates p-type Ni1−xO:Li/n-Si heterojunction solar cells (P+/n HJSCs) by using radio frequency (RF) magnetron sputtering and investigates the effect of substrate temperature on photovoltaic cell properties. Grazing incidence x-ray diffraction, four point probe, and ultraviolet-visible-near infrared discover the optoelectrical properties of p-Ni1-xO thin films. The results show that p-Ni1-xO thin films deposited at 300 oC has the highest grain size (22.4 nm), average visible transmittance (~42%), and electrical resistivity (2.7 Ωcm). However, the conversion efficiency of cell is shown only 2.33% which is lower than the cell (3.39%) fabricated at room temperature. This result can be mainly attributed to interfacial layer thickness (SiOx) reduces from 2.35 nm to 1.70 nm, as verified by high-resolution transmission electron microscopy.