Research methodology and techniques
Two methods of synthesis will be applied: solid phase sintering/crystallization and sol-gel method in order to identify the advantages and disadvantages of obtaining specific mineral phases with certain characteristics. The ratios of the basic oxides of the pyroxene sequences diopside and augite will be specified and a complete series of impurity concentrations will be investigated.
Fully characterized by the obtained ceramics, through the complex of modern analytical methods available at the Institute of mineralogy and crystallography-BAS, University of Ruse and Institute of inorganic chemistry, Rez, Czech Academy of sciences in order to clarify the mechanisms of isomorphic substitution, mechanisms of colour formation, structural and optical properties.
Attempts will be made to incorporate waste materials into the synthesis of new pigment ceramics. The accumulated research experience and the available research infrastructure are a good prerequisite for the successful implementation of the project.
Previous accomplishments and competencies of the research team in the research area of the project
The members of the research team have considerable experience in the synthesis of zirconium, spinel, garnet and wilemite ceramic pigments. Different colours of temperature-resistant ceramic pigments have been obtained, which are characterized by various methods of analysis. The mechanism of pigment formation was studied, crystalchemical analysis is performed and the incorporation of the chromophore ion into the lattice of the basic crystal is clarified. The research team has previous studies on the utilization of waste catalysts from Lukoil Neftochim Burgas/ from hydrotreatment installation for diesel fraction, waste from diesel fractions hydrotreatment plant, waste from solid and heavy waste incineration plant into the synthesis of ceramics. The properties of the obtained pigments were investigated by X-ray phase analysis, infrared spectroscopy, Mössbauer spectroscopy, scanning electron microscopy, colour measurement and more. From the depleted molecular sieves and clays, ceramics in the MnO – ZnO – Al2O3 system are synthesized, the main phases being the minerals gahnite and galaxite from the spinel group. AFM spectroscopy has shown that the synthesized ceramics are smooth. Facade ceramics were obtained with a wide color range from milky white through ochra, light to dark brown coloring using a waste catalyst mass .
Capacity of the applying and partner organizations to conduct the proposed research
The basic organization “Angel Kanchev” Ruse University is institutionally accredited by the National Evaluation and Accreditation Agency (NEAA). The University provides all its resources (laboratories, halls, libraries, software, equipment, etc.) for use by the project team in accordance with the requirements of the work program. The scientific research sector at the University provides full financial, accounting and administrative support for the project. “Angel Kanchev” Ruse University has many years of practice in the research work in the field of synthesis of new materials, in particular ceramic materials, glass ceramics, various glasses, composite materials, etc.; mathematical chemistry and informatics; engineering chemistry and fluidized bed technique; biotechnology; industrial management and more.
The “Angel Kanchev” Ruse University has the necessary infrastructure and equipment to perform the tasks described in the project.
The “Angel Kanchev” Ruse University is a leading scientific organization in Northern Bulgaria. The university is among the first in the country in terms of funded research. For example, for the 2018 calendar year the number of contracts serviced by the university is 92, and the funding received from the research activity is BGN 1733719, 90% of which are from contracts with international organizations.
For the fulfillment of the goals and tasks of the project, the team has the following equipment directly related to the implementation of the project: Lovibont Tintometer RT 100 Colour spectrometer for measuring pigment colour coordinates, ball mills with grinders, dry mill materials, laboratory muffle furnaces – 2 pcs.; box furnace to 1200 ⁰С; technical and precision analytical scales; moisture meter Shimadzu, quartz dilatometer; multifunctional magnetic stirrer; spectrophotometric laboratory equipped with a set of spectrophotometers for the spectral range from 0.2 µm to 25 µm by Carl Zeiss, Jena; metallographic microscopes.
The partner organization- Institute of Mineralogy and Crystallography “Acad. Ivan Kostov” – Bulgarian Academy of Sciences is one of the leading scientific organizations in Bulgaria in the field of research of structure, composition, properties, behaviour and the interactions of solid matter –with complex and modern scientific equipment and highly qualified scientific staff. IMC has 8 state-of-the-art laboratories and participation in 3 external ones http://www.imc.bas.bg/bg1/index.php/9-uncategorised/50-labs.
The following equipment available in the IMC (or in a consortium) will be used: CARL ZEISS SMT SEM EVO LS25 Scanning Electron Microscope with WDS spectrometer; Philips EM 420 T Transmission Electron Microscope Philips SEM 515 Scanning Microscope; Oxford Diffraction Supernova single crystal diffractometer; Bruker AXS – D2 Phaser X-ray diffractometer; Empyrean series 3 (Malvern Panalytical) with TTK 600 Low Temperature Chamber (Antoon Paar) and SAXS, Stanton Redcroft STA with DSC 15; DSC 250 TA Instruments, nano ITC TA Affinity 190 ul, Mid and NIR IR spectrometer Tenzor 37, Hyperion 2000 infrared microscope with thermal stage LinkamIR 600; UV/VIS Carry 4000 spectrophotometer, specific surface area analyzer BET Flex 3D (Micromeretics), Dynamic light scattering DLS, x-ray fluorescence WDXRF Supermini 200 (Rigaku) spectrometer, optical microscopes and more.
The working team will have guaranteed free access to the research equipment at the Institute of Mineralogy and Crystallography “Acad. Ivan Kostov” and “Angel Kanchev” University of Ruse.
For the purposes of the project, it is planned to purchase a ball mill Model SD / 1-1000 for grinding and homogenizing the raw materials, a set of mortars and balls for grinding and homogenizing and a muffle furnace for synthesizing ceramic pigments at higher temperatures up to 1400oC, which will be owned and located in the Base Organization – “Angel Kanchev” University of Ruse.
Intended for purchase are license and upgrade of the existing software in the Laboratory Spectroscopy of IMC-BAS, sample holders and other parts for the FTIR spectrometer Tensor 37.
Upon completion of the project, the purchased equipment will be used for scientific work and for the work of doctoral students and graduate students at “Angel Kanchev” University of Ruse.
Рaid analyzes in external laboratories include: AFM spectroscopy; EPR spectroscopy, and X-ray emission spectroscopy (XES).