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Research Programmes

 

Synthesis and Analysis of Nanostructures

Prof. RNDr. Jiří Pinkas, Ph.D.
Research Group Leader

THEMATIC RESEARCH FOCUS

RESEARCH AREAS

  • Nonhydrolytic sol-gel syntheses of porous metal oxides, phosphates, silicates, metallo-organic coordination polymers and frameworks, molecular building blocks for metallophosphate materials
  • Sonochemical synthesis of binary and ternary metal oxide nanoparticles and precipitation of nuclear waste forms
  • Nanoparticles of metals and alloys as lead-free solders, calculation and verifi cation of their phase diagrams
  • Theoretical studies of structural, magnetic, thermodynamic properties of intermetallic phases, magnetism of grain boundaries
  • Semiempirical phase equilibria modeling using CALPHAD method
  • Macrocyclic ligands, physico-chemical properties of complexes and application in medicine, radiotherapy, and diagnostics (MRI, PET, SPECT, luminescence probes)
  • Development of sensors and sensor arrays – environmental/in vivo analysis
  • Laser ablation-ICP-MS applications to elemental mapping of corroded layers for structural materials of molten salt reactors (MSR), microanalysis of geological and archaeological samples, microanalysis and elemental mapping of biominerals and biological samples
  • Laser Induced Breakdown Spectroscopy (LIBS) elemental mapping and microanalyses, development of LIBS analytical methods with LA-ICP-OES/MS

MAIN OBJECTIVES

Fabrication of nanostructures by ”bottom-up” methods

Nonhydrolytic sol-gel syntheses of nanoporous metal oxides, phosphates, silicates. Synthesis and assembly of molecular building blocks to new materials. Sonochemical methods of nanoparticle synthesis, synthesis of alloy nanoparticles, synthesis of inorganic-organic complex materials, coordination and modifi ed polymers and supramolecular entities. Surface mounted functional molecules. All the developed methods will be utilised directly for fabrication of nanostructures, advanced materials and devices.

Investigation of the functional properties of nanostructures

Characterisation and optimisation of the functional properties of nanostructures for catalysis, nanoelectronics, nanophotonics and (bio)sensing, their correlation with structural parameters of nanostructures and operational parameters. Theoretical ab initio electronic structure calculations of structural, magnetic, thermodynamic properties of materials. Novel and unique properties of nanostructures not observable at conventional materials and microstructures open the ways for qualitatively new applications.

Research and develepment of submicron devices and nanostructures

Development of the methods and techniques into higher functional integrated systems, optimised nanocatalysts, soldering formulation based on nanoalloy particles, nano- and micro-analytical systems and sensors and advanced materials for them. Nanostructures implemented into these systems will enhance the performance and efficiency of devices and systems and widen the areas of their applications e.g. in catalysis, separation, soldering, mapping and imaging, biosensing, biorecognition.

Research and development of analytical and measurement methods

Development of the techniques and methodologies for analysis of nanomaterials/nanostructures and for diagnostics of their properties – new techniques of elemental mapping, microanalysis, MS surface imaging, medical diagnostics, biosensing. This will be used for meeting the other objectives of the Advanced Nanotechnologies and Microtechnologies Research Programme and characterisation of nano- and micro-structures in general.

CONTENT OF RESEARCH

Fabrication of nanostructures by bottom-up methods

Sonochemical and thermolytic synthesis of nanomaterials

The preparation of nanomaterials by means of ultrasound and thermolytic methods – synthesis of nanoscopic metals, alloys, metal oxides from newly designed precursors. The study of the mechanisms of sonochemical and thermolytic transformations of molecular precursors to solid state products and the ways of controlling these reactions. Emphasis on gaining control over the chemical constitution, phase composition, and morphology of the synthesised nanoparticles.

Synthesis of inorganic-organic materials – complexes, coordination polymers, modified polymers and supramolecular systems.

The development of methods for the preparation of molecular building blocks for the construction of new functional materials using the bottom-up approach. The complete characterisation of the structure of new molecular species suitable for forming higher molecular, supramolecular, polymeric, and nanostructured systems. Studies of molecular features providing functionalities for binding or cross-linking leading to porous materials, metallo-organic, coordination and organic polymers. Studies of the chemical properties including intermolecular interactions and self-organisation properties. Tuning the physico-chemical properties and experimental conditions influencing precursor reactivity for kinetic control of reactions. The expected applications are aimed mainly at molecular electronics and opto-electronics, nano-additives for polymeric membranes, separation techniques, gas storage, catalysis, sensors in bio-analytical chemistry, self-assembled monolayers, the development of molecular machines, etc.

Investigation of the functional properties of nanostructures

The main goal is to find a correlation between the properties and the geometrical and structural parameters of nanostructures and to use this knowledge for feedback in the technology of their preparation and for various applications.

Theoretical studies of extended defects in metallic materials and of properties of intermetallic phases

  • Theoretical ab initio electronic structure calculations of structure and magnetism of grain boundaries.
  • Theoretical calculations of structural, magnetic, thermodynamic properties of intermetallic phases.
  • Semiempirical phase equilibria modeling using CALPHAD (CALculation of PHAse Diagrams) method, also in nanoparticles and nanowires (nanoalloys).
  • Development and application of ab initio and semiempirical techniques for studies of chemical, mechanical and magnetic properties of extended defects in metallic materials and analysis of the effect of impurity segregation on their strength and ductility. Construction of phase diagrams of systems with complex intermetallic phases by a combination of ab initio electronic calculations and a phenomenological CALPHAD method, also in nanoparticles and nanowires (nanoalloys).

Research and development of instruments and methods for the investigation of nanomaterials and nanostructures

The development of methods and methodologies for the analysis of nanomaterials, nanostructures, for measuring their properties and the development of new analytical/diagnostic equipment and components. To surpass the limits of individual methods and the ambiguities of their results on the local characterisation of individual nanoobjects the combinations of more analytical techniques and procedures will be developed.

Methods, such as desorption mass spectrometry with nanoparticle matrix (MALDI/SALDI TOF MS), high–throughput off-line analysis of microcolumn fractions (CE/HPLC – MALDI TOF MS), simultaneous detection: MALDI/ICP MS, fluorescence, capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) will be developed.

Mass spectrometry imaging and laser ablation-ICP-MS and Laser Induced Breakdown Spectroscopy (LIBS) elemental mapping will be applied to many diverse types of samples, such as corroded layers for structural materials of molten salt reactors (MSR), geological and archaeological samples, biominerals and biological samples.

KEY RESEARCH EQUIPMENT

PLANNED RESEARCH INFRASTRUCTURE

Core Facilities

The research group will be one of the principal users of the equipment available within CEITEC Nanolithography and Nanofabrication and Nanocharacterisation Core Facilities.

Technology Units

NMR and Mass Spectrometry

CURRENT RESEARCH INFRASTRUCTURE

Material synthesis (glove box, ultrasonic processor, tube furnaces, high-pressure autoclaves, microwave reactors); diffraction techniques (single-crystal X-ray diff ractometer at variabl etemperatures); elemental analyses (ICP/OES spectrometer, ICP/MS spectrometer); mass spectrometry (TOF and quadrupole mass spectrometers); vibrational spectroscopy (FT-IR spectrometer, FT-Raman spectrometer); laser ablation systems; molecular spectroscopy (UV/Vis spectrometers, spectrofl uorimeter); nuclear magnetic resonance (solution and solid-state spectroscopy), computer cluster consisting of ten linked computers, codes WIEN2K, VASP and ABINIT.

MAIN PROJECTS

  • Nonhydrolytic Sol-Gel Reactions for the Synthesis of Silicates and Phosphates with Controlled Porosity and Surface Functionality (LH11028), Ministry of Education, Youth and Sports, 2011-2014, J. Pinkas, Masaryk University.
  • Theoretical studies of grain boundaries with point defects and their aggregates (GA202/09/1786), Czech Science Foundation, 2009-2011, M. Šob, Masaryk University, J. Kuriplach, Charles University in Prague.
  • Thermodynamics of intermetallic phases using combined theoretical and experimental approach (GAP108/10/1908), Czech Science Foundation, 2010-2012, J. Pavlů, Masaryk University, A. Kroupa, Institute of Physics of Materials AS CR.
  • Chemical, mineralogical and statistical analysis of set of urinary stones of patients of Ostrava city agglomeration (GA203/09/1394), Czech Science Foundation, 2009-2011, V. Kanicky, Masaryk University, P. Martinec, Institute of Geonics AS CR.
  • Metal Oxides and Phosphates as Nuclear Waste Forms: Sonochemical Precipitation, Thermal Transformations, and Solubility Studies (GAP207/11/0555), Czech Science Foundation, 2011-2013, J. Pinkas, Masaryk University.

SELECTED PUBLICATIONS

  • VSIANSKA, M., SOB, M. The eff ect of segregated sp-impurities on grain-boundary and surface structure, magnetism and embrittlement in nickel. Progr. Mat. Sci. 2011, 56(6), p. 817-840.
  • PAVLU, J., VRESTAL, J. ,SOB, M. Thermodynamic modeling of Laves phases in the Cr_Hf and Cr_Ti systems: Reassessment using fi rst-principles results. CALPHAD. 2010, 34(2), p. 215-221.
  • LEGUT, D., FRIAK, M., SOB, M. Phase stability, elasticity, and theoretical strength of polonium from fi rst principles. Phys. Rev. B. 2010, 81(21), p. 214118(1) -214118(19).
  • JUNGOVA, P., NAVRATILOVA, J., PES, O., VACULOVIC, T., KANICKY, V., SMARDA, J., PREISLER, J. Substrate-assisted laser desorption inductively-coupled plasma mass spectrometry for determination of copper in myeloid leukemia cells. J. Anal. At. Spectrom. 2010, 25(5), p. 662-668.
  • PINKAS, J., REICHLOVA, V., SERAFIMIDISOVA, A., MORAVEC, Z., ZBORIL, R., JANCIK, D., BEZDICKA, P. Sonochemical Synthesis of Amorphous Yttrium Iron Oxides Embedded in Acetate Matrix and their Controlled Thermal Crystallization towards Garnet (Y3Fe5O12) and Perovskite (YFeO3) Nanostructures. J. Phys. Chem. C. 2010, 114(32), p. 13557.