V Georgieva

Gas sensing properties of very thin TiO2 films prepared by atomic layer deposition (ALD)

Very thin titanium dioxide (TiO2) films of less than 10 nm were deposited by atomic layer deposition (ALD) in order to study their gas sensing properties. Applying the quartz crystal microbalance (QCM) method, prototype structures with the TiO2 ALD deposited thin films were tested for sensitivity to NO2. Although being very thin, the films were sensitive at room temperature and could register low concentrations as 50-100 ppm. The sorption is fully reversible and the films seem to be capable to detect for long term. These initial results for very thin ALD deposited TiO2 films give a promising approach for producing gas sensors working at room temperature on a fast, simple and cost-effective technology.

The surface parameters modifications at nano scale for biomedical applications

Functional coatings deposition is an effective way of surface modification with direct control of stoichiometry, impurity elements, functional groups and surface charges. Modified surface properties such as composition, roughness, wettability have effect on the most important processes at biomaterial interface. The aim of present study was the analysis of surface roughness and surface free energy parameters of oxide Al2O3 and Ta2O5 coatings and the possibility to separate the influence of such factors on the regularities and mechanisms of nano materials interactions with the biological objects.

Comparative analysis of electrophysical properties of ceramic tantalum pentoxide coatings, deposited by electron beam evaporation and magnetron sputtering methods

Ta2O5 ceramic coatings have been deposited on glass substrates by e-beam evaporation and magnetron sputtering methods. For the magnetron sputtering process Ta target was used. X-ray diffraction measurements show that these coatings are amorphous. XPS survey spectra of the ceramic Ta2O5 coatings were obtained. All spectra consist of well-defined XPS lines of Ta 4f, 4d, 4p and 4s; O 1s; C 1s. Ta 4f doublets are typical for Ta2O5 coatings with two main peaks. Scanning electron microscopy and atomic force microscopy images of the e-beam evaporated and magnetron sputtered Ta2O5 ceramic coatings have revealed a relatively flat surface with no cracks. The dielectric properties of the tantalum pentoxide coatings have been investigated in the frequency range of 100 Hz to 1 MHz. The electrical behaviour of e-beam evaporated and magnetron sputtered Ta2O5 ceramic coatings have also been compared. The deposition process conditions principally effect the structure parameters and electrical properties of Ta2O5 ceramic coatings. The coatings deposited by different methods demonstrate the range of dielectric parameters due to the structural and stoichiometric composition changes

Study of quartz crystal microbalance NO2 sensor coated with sputtered indium tin oxide film

A study of NO2 gas sorption ability of thin indium tin oxide (ITO) deposited on 16 MHz quartz crystal microbalance (QCM) is presented. ITO films are grown by RF sputtering of indium/tin target with weight proportion 95:5 in oxygen environment. The ITO films have been characterized by X-ray photoelectron spectroscopy measurements. The ITO surface composition in atomic % is defined to be: In-40.6%, Sn-4.3% and O-55%. The thickness and refractive index of the films are determined by ellipsometric method. The frequency shift of QCM-ITO is measured at different NO2 concentrations. The QCM-ITO system becomes sensitive at NO2 concentration ≥ 500 ppm. The sorbed mass for each concentration is calculated according the Sauerbrey equation. The results indicated that the 1.09 ng of the gas is sorbed into 150 nm thick ITO film at 500 ppm NO2 concentration. When the NO2 concentration increases 10 times the calculated loaded mass is 5.46 ng. The sorption process of the gas molecules is defined as reversible. The velocity of sorbtion /desorption processes are studied, too. The QCM coated with thin ITO films can be successfully used as gas sensors for detecting NO2 in the air at room temperature.

Quartz roughness affect on W03 coated QCM

The influence of the initial quartz roughness on the WO3-QCM (Quartz Crystal Microbalance) parameters and sorption properties was investigated. Experiments were carried out using AT-cut quartz crystal with different surface roughness obtained after treatment with SiC abrasive having grain size of 3 μm, 7 μm, 14 μm and 20 μm respectively. The QCMs were covered with thin WO3 films. The equivalent dynamic parameters of the WO3- QCM were measured and a correlation with the surface roughness was determined. The equivalent dynamic resistance of the as-created QCM increases from 15.42 Ω to 117 Ω and the quality factor decreases as a result of the roughness changes. The surface morphology was observed by a Scanning Electron Microscopy (SEM), which showed higher increase of the WO3 surface roughness compared to those of the initial quartz surface. The cross-section profiles of the investigated structures show different overlay of Au-electrodes. The sorption properties of WO3-QCM system to NH3 were studied in the range from 10 ppm to 1000 ppm. The response and recovering times were determined. The experimental results show an increase of the sorption ability with the increase of the initial quartz roughness. By increasing the roughness the mass-loading is improved.

Liquid Phase Deposition Of Thin Titanium Dioxide Films For NH3 Detection

TiO2 thin films are prepared by a new method called Liquid Phase Deposition (LDP). The layers are obtained by the reaction between the metal fluorocomplex and boric acid in aqueous solution. The morphology of the films and the composition are investigated by scanning electron microscopy (SEM) and x‐ray photoelectron spectrometry (XPS). The sorption properties of TiO2 film to NH3 are measured by the Quartz Crystal Microbalance (QCM) method. A correlation between NH3 concentration and the sorption ability of as‐deposited and annealed samples is obtained.

Laser-induced electron transfer desorption/ionization of metal complexes on TiO2 films

Thin titanium dioxide (TiO2) films were studied as ion emitters for the laser-induced electron transfer desorption/ionization (LETDI) of metal complexes with organic reagents. The TiO2 films (350 nm thick) were deposited on the silicon substrates by e-beam evaporation of TiO2 powder. Copper complex with phthalocyanine, rhenium complex with thiocarbanilide and platinum complex with 8-quinolinethiol were studied as the test analytes. Reflectron time-of- flight mass spectrometer with the rotating ball interface was used for analysis. The analytes were applied on the surface of TiO2 film using an electrospray deposition. All tested compounds are detected as the radical molecular ions with no fragmentation. It is found, that TiO2 films are very stable and show good sensitivity in examined range of the analyte concentrations. The limits of detection of studied complexes were at the subfemtomole range, and the relative standard deviation was less than 10%.

Application of electrochemically deposited nanostructured ZnO layers on quartz crystal microbalance for NO2 detection

The research was fixed on sensing behavior of ZnO nanostructured (NS) films to NO2 concentrations in the environment. The ZnO NS layers are deposited by electrochemical method on quartz resonators with Au electrodes. The sorption properties of ZnO layers were defined by measuring the resonant frequency shift (Δf) of the QCM-ZnO structure for different NO2 concentrations. The measurements were based on the correlation between the frequency shift of the QCM and additional mass loading (Δm) on the resonator calculated using Sauerbrey equation for the AT-cut quartz plate. Frequency – Time Characteristics (FTCs) of the samples were measured as a function of different NO2 concentrations in order to define the sorption abilities of ZnO layers. The experiments were carried out on a special set up in a dynamical regime. From FTCs the response and the recovery times of the QCM-ZnO structure were measured with varying NO2. Frequency shift changed from 23 Hz to 58Hz when NO2 was varied in the range of 250ppm – 5000ppm. The process of sorption was estimated as reversible and the sorption as physical. The obtained results demonstrated that QCM covered with the electrochemically deposited nanostructured ZnO films can be used as application in NO2 sensors.

Modification of the structure and composition of Ca10(PO4)6(OH)2 ceramic coatings by changing the deposition conditions in O2 and Ar

Hydroxyapatite Ca10(PO4)6(OH)2 (HAp) is a material considered to be used to form structural matrices in the mineral phase of bone, dentin and enamel. HAp ceramic materials and coatings are widely applied in medicine and dentistry because of their ability to increase the tissue response to the implant surface and promote bone ingrowth and osseoconduction processes. The deposition conditions affect considerably the structure and bio-functionality of the HAp coatings. We focused our research on developing deposition methods allowing a precise control of the structure and stoichiometric composition of HAp thin films. We found that the use of O2 as a reactive gas improves the quality of the sputtered hydroxyapatite coatings by resulting in the formation of films of better stoichiometry with a fine crystalline structure.

Improving Resonance Characteristics of Gas Sensors by Chemical Etching of Quartz Plates

The paper presents the results of the influence of the etching process of AT-cut quartz plates on the resonance parameters and the QCM sensors. Quartz wafers (100 μm thick, with a diameter of 8 mm), divided into five groups, have been etched in [NH4]2 F2: H2O = 1:1 solution at temperatures in the range from 70°C to 90°C. The influence of etching temperature on the surface morphology of quartz wafers has been estimated by Atomic Force Microscopy (AFM). A correlation between the etching temperature and the dynamic characteristics is obtained. The optimal etching conditions for removing the surface damages caused by the mechanical treatment of the quartz wafers and for obtaining a clean surface were determined. The typical parameters of fabricated resonators on the quartz plates etched in the temperature range from 70°C to 90°C are as follows: Frequency, Fs 16 MHz ± 100 kHz Motional resistance, Rs less 10 Ω Motional inductance, Lq higher than 3 mH Motional capacitance, Cq less 30 fF Static capacitance, Co around 5 pF Quality factor, Q from 46 000 to 70 000 Sorption properties of QCM – MoO3 are evaluated at NH3 concentrations in the interval from 100 ppm to 500 ppm.