Yuri I. Golovin

Zirconia nanofiber mats containing filaments with the average diameter of less than 100 nm were fabricated. It is found that the hardness and Young’s modulus of the mats are sensitive to the microstructure, phase composition and average diameter of the zirconia nanofibers. The hardness and Young’s modulus of the prepared zirconia nanofiber mats vary from 0.86 to 1.67 MPa and from 133 to 362 MPa, respectively, wherein an increase in hardness is accompanied by the rise in Young’s modulus.

Wet high-energy milling and uniaxial pressing are used to fabricate CaO-stabilized tetragonal zirconia polycrystalline ceramic (Ca-TZP) with decent mechanical characteristics, i.e., a hardness of 11.5 GPa, Young’s modulus of 230 GPa, and fracture toughness of 13 MPa·m^0.5. The effect of CaO concentration and the sintering temperature on phase composition and mechanical characteristics of CaO-stabilized zirconia ceramic made of baddeleyite is investigated.

The mats of yttria-stabilized tetragonal zirconia nanofibers were prepared using electrospinning. The effect of calcination temperature in the range of 600–1200 °C on their microstructure, phase composition and mechanical properties was investigated. Phase composition of the nanofibers did not change in all ranges of the calcination temperatures, while the average grain size increased from 8 to 39 nm. Nanoindentation testing of the mats showed a decrease in the hysteresis loop energy in samples with higher calcination temperature. Hardness and the elastic modulus measured with the indentation technique were the highest for the mats calcined at 900 °C.

For the first time, dense nanofibers of yttria-stabilized tetragonal zirconia with diameter of ca. 140 nm were prepared by calcination of electrospun zirconium acetylacetonate/yttrium nitrate/polyacrylonitrile fibers at 1100–1300 °C. Ceramic filaments were characterized by scanning electron microscopy, X-ray diffractometry, and nitrogen adsorption. With a rise in the calcination temperature from 1100 to 1300 °C, the fine-grain structure of the nanofibers transformed to coarse-grain ones with the grain size equal to the fiber diameter. It was revealed that fully tetragonal nanofibrous zirconia may be obtained at Y₂O₃ concentrations in the range of 2–3 mol% at all used calcination temperatures. The addition of 2–3 mol% yttria to zirconia inhibited ZrO₂ grain growth, preventing nanofibers’ destruction at high calcination temperatures. Synthesized well-sintered, non-porous, yttria-stabilized tetragonal zirconia nanofibers can be considered as a promising material for composites’ reinforcement, including composites with ceramic matrix.

For the first time, zirconia nanofibers with an average diameter of about 75 nm have been fabricated by calcination of electrospun zirconium acetylacetonate/polyacrylonitrile fibers in the range of 500–1100 °C. Composite and ceramic filaments have been characterized by scanning electron microscopy, thermogravimetric analysis, nitrogen adsorption analysis, energy-dispersive X-ray spectroscopy, and X-ray diffractometry. The stages of the transition of zirconium acetylacetonate to zirconia have been revealed. It has been found out that a rise in calcination temperature from 500 to 1100 °C induces transformation of mesoporous tetragonal zirconia nanofibers with a high specific surface area (102.3 m²/g) to non-porous monoclinic zirconia nanofibers of almost the same diameter with a low value of specific surface area (8.3 m²/g). The tetragonal zirconia nanofibers with high specific surface area prepared at 500 °C can be considered, for instance, as promising supports for heterogeneous catalysts, enhancing their activity.

A set of new approaches and techniques of non-destructive testing is described and implemented within a unified computer analysis of the patterns of multi-scale dynamic thermography. Depending on the size of the inspected area, nature, location, orientation and size of the defects, various energy sources were used for probe dynamic heating of the controlled article: air flow, focused laser beam, and point contact. The non-stationary thermal picture of the monitored area was recorded with a high resolution thermal imaging device and then analyzed using original model approaches and developed software. A set of discussed approaches allows detecting and quantitative characterizing of the defects of various types, size (from fractions to tens of millimeters) and orientation, including cracks, coating delamination or degradation, welding and glue seams defects, deposits, etc., both at the outer and inner surfaces of tubes, tanks, and reactors, etc. The developed methods provides determination of the thermophysical characteristics of the material, i.e., the thermal diffusivity coefficient with an accuracy better than ±3%.