The Influence of Annealing on the Optical Properties and Microstructure Recrystallization of the TiO2 Layers Produced by Means of the E-BEAM Technique

Titanium dioxide films, about 200 nm in thickness, were deposited using the e-BEAM technique at room temperature and at 227 °C (500K) and then annealed in UHV conditions (as well as in the presence of oxygen (at 850 °C). The fabricated dielectric films were examined using X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, scanning electron microscopy, transmission electron microscopy, and spectroscopic ellipsometry. The applied experimental techniques allowed us to characterize the phase composition and the phase transformation of the fabricated TiO₂ coatings. The films produced at room temperature are amorphous but after annealing consist of anatase crystallites. The layers fabricated at 227 °C contain both anatase and rutile phases. In this case the anatase crystallites are accumulated near the substrate interface whilst the rutile crystallites were formed closer to the surface of the TiO₂ film. It should be emphasized that these two phases of TiO₂ are distinctly separated from each other.     

Biocompatibility and Surface Properties of TiO2 Thin Films Deposited by DC Magnetron Sputtering

We present the study of the biocompatibility and surface properties of titanium dioxide (TiO₂) thin films deposited by direct current magnetron sputtering. These films are deposited on a quartz substrate at room temperature and annealed with different temperatures (100, 300, 500, 800 and 1100 °C). The biocompatibility of the TiO₂ thin films is analyzed using primary cultures of dorsal root ganglion (DRG) of Wistar rats, whose neurons are incubated on the TiO₂ thin films and on a control substrate during 18 to 24 h. These neurons are activated by electrical stimuli and its ionic currents and action potential activity recorded. Through X-ray diffraction (XRD), the surface of TiO₂ thin films showed a good quality, homogeneity and roughness. The XRD results showed the anatase to rutile phase transition in TiO₂ thin films at temperatures between 500 and 1100 °C. This phase had a grain size from 15 to 38 nm, which allowed a suitable structural and crystal phase stability of the TiO₂ thin films for low and high temperature. The biocompatibility experiments of these films indicated that they were appropriated for culture of living neurons which displayed normal electrical behavior.     

Sol-Gel Synthesis and Antioxidant Properties of Yttrium Oxide Nanocrystallites Incorporating P-123

Yttrium oxide (Y₂O₃) nanocrystallites were synthesized by mean of a sol-gel method using two different precursors. Raw materials used were yttrium nitrate and yttrium chloride, in methanol. In order to promote oxygen vacancies, P-123 poloxamer was incorporated. Synthesized systems were heat-treated at temperatures from 700 °C to 900 °C. Systems at 900 °C were prepared in the presence and absence of P-123 using different molar ratios (P-123:Y = 1:1 and 2:1). Fourier transform infrared spectroscopy (FTIR) results revealed a characteristic absorption band of Y–O vibrations typical of Y₂O₃ matrix. The structural phase was analyzed by X-ray diffraction (XRD), showing the characteristic cubic phase in all systems. The diffraction peak that presented the major intensity corresponded to the sample prepared from yttrium chloride incorporating P-123 in a molar ratio of P-123:Y = 2:1 at 900 °C. Crystallites sizes were determined by Scherrer equation as between 21 nm and 32 nm. Antioxidant properties were estimated by 2,2-diphenyl-1-picrylhydrazyl (DPPH•) assays; the results are discussed.     

Photocatalytic Oxidation of Low-Level Airborne 2-Propanol and Trichloroethylene over Titania Irradiated with Bulb-Type Light-Emitting Diodes

This study examined the photocatalytic oxidation of gas-phase trichloroethylene (TCE) and 2-propanol, at indoor levels, over titanium dioxide (TiO₂) irradiated with light-emitting diodes (LED) under different operational conditions. TiO₂ powder baked at 450 °C exhibited the highest photocatalytic decomposition efficiency (PDE) for TCE, while all photocatalysts baked at different temperatures showed similar PDEs for 2-propanol. The average PDEs of TCE over a three hour period were four, four, five, and 51% for TiO₂ powders baked at 150, 250, 350, and 450 °C, respectively. The average PDEs of 2-propanol were 95, 97, 98, and 96% for TiO₂ powders baked at 150, 250, 350, and 450 °C, respectively. The ratio of anatase at 2θ = 25.2° to rutile at 2θ = 27.4° was lowest for the TiO₂ powder baked at 450 °C. Although the LED-irradiated TiO₂ system revealed lower PDEs of TCE and 2-propanol when compared to those of the eight watt, black-light lamp-irradiated TiO₂ system, the results for the PDEs normalized to the energy consumption were reversed. Other operational parameters, such as relative humidity, input concentrations, flow rate, and feeding type were also found to influence the photocatalytic performance of the UV LED-irradiated TiO₂ system when applied to the cleaning of TCE and 2-propanol at indoor air levels.     

Effect of Calcination Temperature and Chemical Composition of PAN-Derived Carbon Microfibers on N2, CO2, and CH4 Adsorption

This work investigates the interplay of carbonization temperature and the chemical composition of carbon microfibers (CMFs), and their impact on the equilibration time and adsorption of three molecules (N₂, CO₂, and CH₄). PAN derived CMFs were synthesized by electrospinning and calcined at three distinct temperatures (600, 700 and 800 °C), which led to samples with different textural and chemical properties assessed by FTIR, TGA/DTA, XRD, Raman, TEM, XPS, and N₂ adsorption. We examine why samples calcined at low/moderate temperatures (600 and 700 °C) show an open hysteresis loop in nitrogen adsorption/desorption isotherms at −196.15 °C. The equilibrium time in adsorption measurements is nearly the same for these samples, despite their distinct chemical compositions. Increasing the equilibrium time did not allow for the closure of the hysteresis loop, but by rising the analysis temperature this was achieved. By means of the isosteric enthalpy of adsorption measurements and ab initio calculations, adsorbent/adsorbate interactions for CO₂, CH₄ and N₂ were found to be inversely proportional to the temperature of carbonization of the samples (CMF-600 > CMF-700 > CMF-800). The enhancement of adsorbent/adsorbate interaction at lower carbonization temperatures is directly related to the presence of nitrogen and oxygen functional groups on the surface of CMFs. Nonetheless, a higher concentration of heteroatoms also causes: (i) a reduction in the adsorption capacity of CO₂ and CH₄ and (ii) open hysteresis loops in N₂ adsorption at cryogenic temperatures. Therefore, the calcination of PAN derived microfibers at temperatures above 800 °C is recommended, which results in materials with suitable micropore volume and a low content of surface heteroatoms, leading to high CO₂ uptake while keeping acceptable selectivity with regards to CH₄ and moderate adsorption enthalpies.     

Hysteresis in Lanthanide Zirconium Oxides Observed Using a Pulse CV Technique and including the Effect of High Temperature Annealing

A powerful characterization technique, pulse capacitance-voltage (CV) technique, was used to investigate oxide traps before and after annealing for lanthanide zirconium oxide thin films deposited on n-type Si (111) substrates at 300 °C by liquid injection Atomic Layer Deposition (ALD). The results indicated that: (1) more traps were observed compared to the conventional capacitance-voltage characterization method in LaZrO_x; (2) the time-dependent trapping/de-trapping was influenced by the edge time, width and peak-to-peak voltage of a gate voltage pulse. Post deposition annealing was performed at 700 °C, 800 °C and 900 °C in N₂ ambient for 15 s to the samples with 200 ALD cycles. The effect of the high temperature annealing on oxide traps and leakage current were subsequently explored. It showed that more traps were generated after annealing with the trap density increasing from 1.41 × 10¹² cm⁻² for as-deposited sample to 4.55 × 10¹² cm⁻² for the 800 °C annealed one. In addition, the leakage current density increase from about 10⁻⁶ A/cm² at V_g = +0.5 V for the as-deposited sample to 10⁻³ A/cm² at V_g = +0.5 V for the 900 °C annealed one.     

Effect of Heating Modes on Reactive Sintering of Ca3Co4O9 Ceramics

The traditional solid-state reaction method was employed to synthesize bulk calcium cobaltite (Ca349/Ca₃Co₄O₉) ceramics via ball milling the precursor mixture. The samples were compacted using conventional sintering (CS) and spark plasma sintering (SPS) at 850, 900, and 950 °C. The X-ray diffraction (XRD) pattern indicates the presence of the Ca349 phase for samples sintered at 850 and 900 °C. In addition, SPS fosters higher densification (81.18%) than conventional sintering (50.76%) at elevated sintering temperatures. The thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA) performed on the precursor mixture reported a weight loss of ~25.23% at a temperature range of 600–820 °C. This current work aims to analyze the electrical properties (Seebeck coefficient (s), electrical resistivity (ρ), and power factor) of sintered samples as a function of temperature (35–500 °C). It demonstrates that the change in sintering temperature (conventional sintering) did not evince any significant change in the Seebeck coefficient (113–142 μV/K). However, it reported a low resistivity of 153–132 μΩ-m and a better power factor (82–146.4 μW/mK²) at 900 °C. On the contrary, the SPS sintered samples recorded a higher Seebeck coefficient of 121–181 μV/K at 900 °C. Correspondingly, the samples sintered at 950 °C delineated a low resistivity of 145–158 μΩ-m and a better power factor (97–152 μW/mK²).     

Development of Ni-Sr(V,Ti)O3-δ Fuel Electrodes for Solid Oxide Fuel Cells

A series of strontium titanates-vanadates (STVN) with nominal cation composition Sr_1-xTi_1-y-zV_yNi_zO_3-δ (x = 0–0.04, y = 0.20–0.40 and z = 0.02–0.12) were prepared by a solid-state reaction route in 10% H₂–N₂ atmosphere and characterized under reducing conditions as potential fuel electrode materials for solid oxide fuel cells. Detailed phase evolution studies using XRD and SEM/EDS demonstrated that firing at temperatures as high as 1200 °C is required to eliminate undesirable secondary phases. Under such conditions, nickel tends to segregate as a metallic phase and is unlikely to incorporate into the perovskite lattice. Ceramic samples sintered at 1500 °C exhibited temperature-activated electrical conductivity that showed a weak p(O₂) dependence and increased with vanadium content, reaching a maximum of ~17 S/cm at 1000 °C. STVN ceramics showed moderate thermal expansion coefficients (12.5–14.3 ppm/K at 25–1100 °C) compatible with that of yttria-stabilized zirconia (8YSZ). Porous STVN electrodes on 8YSZ solid electrolytes were fabricated at 1100 °C and studied using electrochemical impedance spectroscopy at 700–900 °C in an atmosphere of diluted humidified H₂ under zero DC conditions. As-prepared STVN electrodes demonstrated comparatively poor electrochemical performance, which was attributed to insufficient intrinsic electrocatalytic activity and agglomeration of metallic nickel during the high-temperature synthetic procedure. Incorporation of an oxygen-ion-conducting Ce_0.9Gd_0.1O_2-δ phase (20–30 wt.%) and nano-sized Ni as electrocatalyst (≥1 wt.%) into the porous electrode structure via infiltration resulted in a substantial improvement in electrochemical activity and reduction of electrode polarization resistance by 6–8 times at 900 °C and ≥ one order of magnitude at 800 °C.     

Improvement of La0.8Sr0.2MnO3−δ Cathode Material for Solid Oxide Fuel Cells by Addition of YFe0.5Co0.5O3

The high efficiency of solid oxide fuel cells with La_0.8Sr_0.2MnO_3−δ (LSM) cathodes working in the range of 800–1000 °C, rapidly decreases below 800 °C. The goal of this study is to improve the properties of LSM cathodes working in the range of 500–800 °C by the addition of YFe_0.5Co_0.5O₃ (YFC). Monophasic YFC is synthesized and sintered at 950 °C. Composite cathodes are prepared on Ce_0.8Sm_0.2O_1.9 electrolyte disks using pastes containing YFC and LSM powders mixed in 0:1, 1:19, and 1:1 weight ratios denoted LSM, LSM1, and LSM1, respectively. X-ray diffraction patterns of tested composites reveal the presence of pure perovskite phases in samples sintered at 950 °C and the presence of Sr₄Fe₄O₁₁, YMnO₃, and La_0.775Sr_0.225MnO_3.047 phases in samples sintered at 1100 °C. Electrochemical impedance spectroscopy reveals that polarization resistance increases from LSM1, by LSM, to LSM2. Differences in polarization resistance increase with decreasing operating temperatures because activation energy rises in the same order and equals to 1.33, 1.34, and 1.58 eV for LSM1, LSM, and LSM2, respectively. The lower polarization resistance of LSM1 electrodes is caused by the lower resistance associated with the charge transfer process.     

Synthesis and Tribological Characterization of Ti3SiC2/ZnO Composites

Dense Ti₃SiC₂/ZnO composites were sintered at different temperatures by spark plasma sintering (SPS). The effects of sintering temperature on composition and mechanical properties of Ti₃SiC₂/ZnO composites were studied. The tribological behaviors of Ti₃SiC₂/ZnO composites/Inconel 718 alloy tribo-pairs at elevated temperature from 25 °C to 800 °C were discussed. The experimental results showed that the initial decomposition temperature of the Ti₃SiC₂/ZnO composite was 1150 °C, and Ti₃SiC₂ decomposed into TiC. When the decomposition temperature was higher than 1150 °C, the compositions of the Ti₃SiC₂/ZnO composites were Ti₃SiC₂, ZnO, and TiC. It was found that Ti₃SiC₂/ZnO composites had better self-lubricating performance than Ti₃SiC₂ at elevated temperature from 600 °C to 800 °C, which was owing to material transfers of tribo-pairs and sheared oxides generated by tribo-oxidation reactions.     

Improvement of Corrosion Resistance of TiO2 Layers in Strong Acidic Solutions by Anodizing and Thermal Oxidation Treatment

By anodization and thermal oxidation at 600 °C, an oxide layer on Ti with excellent corrosion resistance in strong acid solutions was prepared. The structural properties of TiO₂ films before and after thermal oxidation were investigated with methods of Scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The electrochemical characterization was recorded via electrochemical impedance spectroscopy, potentiodynamic polarization and Mott–Schottky methods. XRD results show that a duplex rutile/anatase structure formed after oxidation, and the amount of anatase phase increased as the treatment time was prolonged from 3 to 9 h. XPS analysis indicates that as the thermal oxidation time increased, more Ti vacancies were present in the titanium oxide films, with decreased donor concentration. Longer thermal oxidation promoted the formation of hydroxides of titanium on the surface, which is helpful to improve the passive ability of the film. The anodized and thermally oxidized Ti samples showed relatively high corrosion resistance in 4 M HCl and 4 M H₂SO₄ solutions at 100 ± 5 °C. The passive current density values of the thermally oxidized samples were five orders of magnitude under the testing condition compared with that of the anodized sample. With the oxidation time prolonged, the passive current density decreased further to some extent.     

Self-Healing of SiC-Al2O3-B4C Ceramic Composites at Low Temperatures

Self-healing ceramics have been researched at high temperatures, but few have been considered at lower temperatures. In this study, SiC-Al₂O₃-B₄C ceramic composite was compacted by spark plasma sintering (SPS). A Vickers indentation was introduced, and the cracks were healed between 600 °C and 800 °C in air. Cracks could be healed completely in air above 700 °C. The ceramic composite had the best healing performance at 700 °C for 30 min, recovering flexural strength of up to 94.2% of the original. Good crack-healing ability would make this composite highly useful as it could heal defects and flaws autonomously in practical applications. The healing mechanism was also proposed to be the result of the oxidation of B₄C.     

In-Situ Synthesis,Microstructure, and Mechanical Properties of TiB2-Reinforced Fe-Cr-Mn-Al Steel Matrix Composites Prepared by Spark Plasma Sintering

In-situ synthesis, microstructure, and mechanical properties of four TiB₂-Reinforced Fe-Cr-Mn-Al Steel Matrix Composites have been researched in this work. The microstructure and phases of the prepared specimens have been characterized by using scanning electron microscopy (SEM), X-ray diffraction technique, and transmission electron microscopy (TEM). The sintered specimens consisted of Fe₂AlCr, CrFeB-type boride, and TiB₂. The mechanical properties, such as hardness and compression strength at room temperature (RT) and at elevated temperatures (600 °C and 800 °C) have been evaluated. The compressive strength and Vickers hardness of the sintered specimens increase with the volume fraction of TiB₂ in the matrix, which are all much higher than those of the ex-situ TiB₂/Fe-15Cr-20Mn-8Al composites and the reported TiB₂/Fe-Cr composites with the same volume fraction of TiB₂. The highest Vickers hardness and compressive strength at room temperature are 1213 ± 35 HV and 3500 ± 20 MPa, respectively. As the testing temperature increases to 600 °C, or even 800 °C, these composites still show relatively high compressive strength. Precipitation strengthening of CrFeB and in-situ synthesis of TiB₂ as well as nanocrystalline microstructure produced by the combination of mechanical alloying (MA) and spark plasma sintering (SPS) can account for the high Vickers hardness and compressive strength.     

A Comparative Study of the Sintering Behavior of Pure and Manganese-Substituted Hydroxyapatite

Hydroxyapatite (HA) is a widely studied biomaterial for its similar chemical composition to bone and its osteoconductive properties. The crystal structure of HA is flexible, allowing for a wide range of substitutions which can alter bioactivity, biodegradation, and mechanical properties of the substituted apatite. The thermal stability of a substituted apatite is an indication of its biodegradation in vivo. In this study, we investigated the thermal stability and mechanical properties of manganese-substituted hydroxyapatite (MnHA) as it is reported that manganese can enhance cell attachment compared to pure HA. Pure HA and MnHA pellets were sintered over the following temperature ranges: 900 to 1300 °C and 700 to 1300 °C respectively. The sintered pellets were characterized via density measurements, mechanical testing, X-ray diffraction, and field emission electron microscopy. It was found that MnHA was less stable than HA decomposing around 800 °C compared to 1200 °C for HA. The flexural strength of MnHA was weaker than HA due to the decomposition of MnHA at a significantly lower temperature of 800 °C compared to 1100 °C for HA. The low thermal stability of MnHA suggests that a faster in vivo dissolution rate compared to pure HA is expected.     

The Effect of Temperature and Sputtered Particles on the Wettability of Al/Al2O3

Two kinds of Al₂O₃ ceramic samples with and without Al film deposited were designed respectively. The influences of temperature and high kinetic energy sputtering particles on the wettability and interface strength of Al/Al₂O₃ were studied by comparing the wetting behavior of molten aluminum on two samples. The results show that molten aluminum does not wet the Al₂O₃ sample without Al film deposited at 700 °C, the contact angle is 165°, and the interfacial shear strength is 28 MPa. With the increase of temperature, the contact angle decreases continuously, and the interface shear strength gradually increases. The fracture of the brazed joint is transferred from the interface to the brazing seam. In comparison, the sample deposited with Al film is wetted by molten aluminum at 700 °C, and the contact angle is only 12°. The interface shear strength is about 120 MPa and is less affected by temperature. The shear fracture of the joint occurs in the brazed seam of Al metal. Therefore, the high energy generated by either the temperature increase or the particle sputtering enable the Al atoms to overcome the energy barrier to form Al–O bonds with the O atoms on the Al₂O₃ ceramic surface, thereby improving the wettability of Al/Al₂O₃.     

Transforming Pt-SnO2 Nanoparticles into Pt-SnO2 Composite Nanoceramics for Room-Temperature Hydrogen-Sensing Applications

Many low-dimensional nanostructured metal oxides (MOXs) with impressive room-temperature gas-sensing characteristics have been synthesized, yet transforming them into relatively robust bulk materials has been quite neglected. Pt-decorated SnO₂ nanoparticles with 0.25–2.5 wt% Pt were prepared, and highly attractive room-temperature hydrogen-sensing characteristics were observed for them all through pressing them into pellets. Some pressed pellets were further sintered over a wide temperature range of 600–1200 °C. Though the room-temperature hydrogen-sensing characteristics were greatly degraded in many samples after sintering, those samples with 0.25 wt% Pt and sintered at 800 °C exhibited impressive room-temperature hydrogen-sensing characteristics comparable to those of their counterparts of as-pressed pellets. The variation of room-temperature hydrogen-sensing characteristics among the samples was explained by the facts that the connectivity between SnO₂ grains increases with increasing sintering temperature, and Pt promotes oxidation of SnO₂ at high temperatures. These results clearly demonstrate that some low-dimensional MOX nanocrystals can be successfully transformed into bulk MOXs with improved robustness and comparable room-temperature gas-sensing characteristics.     

Preparation and Properties of (YCa)(TiMn)O3?δ Ceramics Interconnect of Solid Oxide Fuel Cells

(YCa)(TiMn)O_3–δ ceramics prepared using a reaction-sintering process were investigated. Without any calcination involved, the mixture of raw materials was pressed and sintered directly. Y₂Ti₂O₇ instead of YTiO₃ formed when a mixture of Y₂O₃ and TiO₂ with Y/Ti ratio 1/1 were sintered in air. Y₂Ti₂O₇, YTiO_2.085 and some unknown phases were detected in Y_0.6Ca_0.4Ti_0.6Mn_0.4O_3–δ. Monophasic Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ ceramics were obtained after 1400–1500 °C sintering. Dense Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ with a density 4.69 g/cm³ was observed after 1500 °C/4 h sintering. Log σ for Y_0.6Ca_0.4Ti_0.6Mn_0.4O_3–δ increased from –3.73 Scm^–1 at 350 °C to –2.14 Scm^–1 at 700 °C. Log σ for Y_0.6Ca_0.4Ti_0.4Mn_0.6O_3–δ increased from –2.1 Scm^–1 at 350 °C to –1.36 Scm^–1 at 700 °C. Increasing Mn content decreased activation energy E_a and increased electrical conductivity. Reaction-sintering process is proved to be a simple and effective method to obtain (YCa)(TiMn)O_3–δ ceramics for interconnects in solid oxide fuel cells.     

Microwave and Terahertz Properties of Spark-Plasma-Sintered Zr0.8Sn0.2TiO4 Ceramics

Zr_0.8Sn_0.2TiO₃ (ZST) powders synthesized by solid-state reaction were subject to processing by spark plasma sintering (SPS). A single-phase ceramic with a high relative density of 95.7% and 99.6% was obtained for sintering temperatures of 1150 °C and 1200 °C, respectively, and for a dwell time of 3 min. In order to reduce the oxygen vacancies, as-sintered discs were annealed in air at 1000 °C. The dielectric loss of the annealed samples, expressed by the Q × f product, measured in the microwave (MW) domain, varied between 35 THz and 50 THz. The intrinsic losses (Q × f ~ 60 THz) were derived by using terahertz time-domain spectroscopy (THz-TDS).     

Effects of TiO2 Nanoparticle Addition on Microstructure and Selected Properties of Ag–xTiO2 Composites

The paper presents the results of a study of the microstructure and selected properties of silver-based composites reinforced with TiO₂ nanoparticles, produced by the powder metallurgy method. Pure silver powders were mixed with TiO₂ reinforcement (5 and 10 wt%) and 5 mm steel balls (100Cr6) for 270 min in a Turbula T2F mixer to produce a homogeneous mixture. The composites were made in a rigid die with a single-action compaction press under a pressure of 400 MPa and 500 MPa and then sintered under nitrogen atmosphere at 900 °C. Additionally, to improve the density and mechanical properties of the obtained sinters, double pressing and double sintering operations were conducted. As a result, compacts with a density of 90–94% were obtained. The microstructure of the sintered compacts consists of uniform grains, and the TiO₂ reinforcement phase particles are located on the grain boundaries. There were no discontinuities at the Ag–TiO₂ contact boundary, which was confirmed by SEM and TEM analysis. The use of a higher pressure had a positive effect on the hardness and flexural strength of the tested materials. It was found that the composites with 5 wt% TiO₂ pressed under 500 MPa are characterized by the highest level of mechanical properties. The hardness of these composites is 57 HB, while the flexural strength is 163 MPa.     

Cyclic Oxidation of Titanium Grade 2

This paper presents the results of research into the cyclic oxidation of titanium Grade 2. The value of titanium Grade 2 oxidation activation energy was determined based on an analysis of the Arrhenius diagram. The result was 205.3 kJ/mol. After cyclic oxidation at a temperature of 600 °C, the presence of oxides in an acicular system was observed on the surface. The specimen surface after oxidation at 650 °C was characterised by the presence of fine oxide particles, while after oxidation at 700 °C, the obtained oxide layer was composed of large oxide particles. The layers obtained after oxidation at 600 °C had the lowest thickness (1.26 and 2.12 µm), while those obtained at 700 °C had the highest thickness (5.17 and 9.45 µm). Examination of the phase composition after cyclic oxidation showed that the oxide layers obtained at temperatures of 600, 650 and 700 °C were composed of TiO₂ (rutile) only. No presence of other phases was found. The oxide layers formed in the cyclic oxidation process were characterised by different thicknesses, depending on the oxidation parameters. It was found that cyclic oxidation contributed to a considerable increase in the surface hardness of titanium Grade 2.