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	Institute of Chemical Process Fundamentals ASCR, v.v.i. Prague

Head: J. Pola

Deputy: R. Fajgar

Research staff: V. Drinek, A. Galikova, J. Kupcik, D. Pokorna, M. Urbanova
Part time: P. Stopka

Technical staff: D. Bartlova

PhD student: T. Krenek, V. Jandova

• IR and UV laser induced chemistry
• IR and UV laser chemical vapour deposition of novel polymeric and Si- , Ge- and C-based materials
• IR laser-induced carbothermal reduction of oxides
• IR and UV laser photopolymerization in the gas phase
• UV laser chemical liquid deposition of metal nanosols and nanocomposites
• IR and UV laser induced ablation of polymers
• IR and UV laser deposition of TiO2-based-photocatalysts

New laser induced process for production of novel carbon-based nanomaterials and carbon-based nanomaterials with incorporated Si, N, and B heteroatoms

(J. Pola, joint project with JH IPC, IIC, and Institute of Physics ASCR, supported by ASCR, grant No. IAA400720619)

MW and GW UV laser-induced photolysis of gaseous benzene and acetylene has been demonstrated as a process leading to transient polyacetylenes and cumulenes and yielding nanostructured carbon soot whose properties depend on the precursor. Simultaneous back-side etching of silica adjacent to laser-induced plasma enables to enrich the soot with polyoxocarbosilane [Ref. 10]. This process with gaseous pyridine allows photochemical etching of silica and deposition of composites containing nanodomains of very rare chaoite in amorphous C/Si/O/N phase [Ref. 12]. Similar process conducted in solution with UV laser photolysis of Fe^II acetylacetonate affords deposition of alpha-Fe/polyoxocarbosilane/carbon nanocomposite whose heating allows evolution to alpha-Fe2O3/Polyoxocarbosilane/Carbon Nanocomposite [Ref. 11]. IR laser thermal etching of silicon monoxide [Ref. 9] and silicon dioxide [Ref. 16] with carbonaceous decomposition products of benzene and acetylene leads to deposition of nanosized silicon oxycarbide (prepared for the first time) and Si/C/O/H phase. These processes occur through carbothermal reduction of silicon oxides.

Pyrolytic and photolytic approach for the deposition of novel Si/Ge/C materials

(V. Drinek, joint project with JH IPC, IIC, supported by ASCR, grant No. IAA400720616)

A conventional pyrolysis of a novel precursor - tris(trimethylsilyl)germane at 300-400 ^oC was performed. It resulted in formation of Ge nanowires (NWs) enveloped in Si/C material. Structure of NWs consists of core (crystalline Ge), inner jacket (nanocrystalline Ge) and outer jacket (Si/C) as revealed by HRTEM analysis. In some NWs the core of hexagonal Ge was established. Further heating under vacuum to 900 ^oC led to a complete evaporation of Ge and yielded thin wall Si1-xCx nanotubes. Lengths of nanowires and nanotubes ranged up to several micrometers. Formation of such nanostuctured material is strongly affected by using appropriate substrate and/or its processing prior deposition. [Refs. 1, 2, 5]

Novel preparation and photocatalytic study of titania-based catalysts

(R. Fajgar, supported by NATO collaborative project, project No. CBP.EAP.CLG.982078)

UV laser-induced deposition of TiO2 and Ti/O/Si materials from TiCl4/O2 (or TiCl4/SiCl4/O2 mixtures was studied. Prepared films, deposited on glass substrates were annealed up to 450 ^oC. Photocatalytic activity and hydrophilicity was studied. The films annealed to 350-400 ^oC possess good adhesion to glass substrate and revealed superhydrophilic properties. Deposition in the presence of chromyl chloride results in formation of chromium-doped films. The doped films were analyzed using available spectroscopic, microscopic and diffraction techniques and photocatalytic activity in the visible light was studied.

Laser decomposition of cobalt and nickel carbonyls in the presence of acetylene for preparation of carbon encapsulated metal nanoparticles

(R. Fajgar, joint project with JH IPC, IIC, and Institute of Physics of the ASCR, v.v.i., supported by GACR, grant No. GA203/07/0546)

Mixture of iron pentacarbonyl, cobalt tricarbonyl nitrosyl and acetylene decomposes under UV laser irradiation to form CoFe alloy nanoparticles encapsulated in carbon. Minor products (benzene, vinylacetylene) are formed as a result of acetylene dimerization and trimerization. Analysis of the solid deposit confirmed formation of the amorphous CoFe nanoparticles with diameter 10 nm, encapsulated in the amorphous carbon. The heating of the deposit to 600, 900 and 1150 ^oC results in crystallization of CoFe as syn-wairauite and better encapsulation. Higher temperature (900 ^oC) causes crystallization of the carbon shells and formation of diamond layers, covering the CoFe nanocrystals. Magnetic measurements revealed strong superparamagnetic behaviour of the CoFe nanoparticles at temperatures up to 140 K.

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• Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Lodz, Poland: UV laser-induced crosslinking of polysiloxanes
• Instituto de Estructura de la Materia, CSIC, Madrid, Spain: Studies on IR laser deposition of nanosized metal chalcogenuides and polycarbosilthianes
• National Institute of Advanced Industrial Research and Technology, Tsukuba, Japan: Laser control of organic reactions
• University of Crete, Heraklion, Greece: Laser induced chemical vapour deposition of polycarbosilthianes
• King Fahd University of Petroleum and Minerals, Dhahran, Saudi Arabia: Laser degradation of contaminants in fuel oils
• National Institute for Lasers, Plasma and Radiation Physics, Bucharest, Romania: Laser-induced CVD of Fe/polymer nanocomposites
• Faculty of Technology and Metallurgy, University of St. Cyril & Methodius, Skopje, R. Macedonia: Novel preparation and photocatalytic study of titania-based catalysts

• M.A. Alsunaidi, King Fahd University of Petroleum & Minerals, Dhahran, Saudi Arabia
• J. Blazevska-Gilev, University of St. Cyril & Methodius, Skopje, R. Macedonia
• L. Diaz, Instituto de Estructura de la Materia, CSIC, Madrid, Spain
• M. Marinkovski, University of St. Cyril & Methodius, Skopje, R. Macedonia
• R. Tomovska, University of St. Cyril & Methodius, Skopje, R. Macedonia

Original papers

1. Drinek V., Galikova A., Subrt J., Fajgar R.: Conventional Pyrolysis of [-C≡C-SiMe2-C≡C-GeMe2-]n Polymer Precursor for Si/Ge/C Materials. J. Anal. Appl. Pyrolysis 81(2), 193-198 (2008).

2. Drinek V., Subrt J., Klementova M., Rieder M., Fajgar R.: From Shelled Ge Nanowires to SiC Nanotubes. Nanotechnology 20(3), 035606 (2008).

3. Galikova A., Pola J.: Highly Sensitive TGA Diagnosis of Thermal Behaviour of Laser-Deposited Materials. Thermochim. Acta 473(1-2), 54-60 (2008).

4. Gondal M.A., Masoudi H.M., Pola J.: Laser Photo-Oxidative Degradation of 4,6-Dimethyldibenzothiophene. Chemosphere 71(9), 1765-1768 (2008).

5. Klementova M., Rieder M., Drinek V., Fajgar R., Subrt J.: Structure of Coated Ge-nanowires. Microsc., Microanal. 14(Suppl. 2), 198-199 (2008).

6. Kowalewska A., Kupcik J., Pola J., Stanczyk W.A.: Laser Irradiation of Oligosiloxane Copolymer Thin Films Functionalized with Side Chain Bulky Carbosilane Moieties. Polymer 49(4), 857-866 (2008).

7. Minceva M., Fajgar R., Markovska L., Meshko V.: Comparative Study of Zn²⁺, Cd^2+o, and Pb²⁺ Removal from Water Solution Using Natural Clinoptilolitic Zeolite and Commercial Granulated Activated Carbon. Equilibrium of Adsorption. Sep. Sci.Technol. 43(8), 2117-2143 (2008).

8. Ouchi A., Bastl Z., Bohacek J., Subrt J., Bakardjieva S., Bezdicka P., Pola J.: Room-Temperature Reaction of Laser-Photolytically Generated Te Nanosols with Silver. J. Photochem. Photobiol., A 200(2-3), 187-191 (2008).

9. Pokorna D., Urbanova M., Subrt J., Bastl Z., Pola J.: IR Laser-Induced Carbothermal Reduction of Silicon Monoxide. J. Anal. Appl. Pyrolysis 83(2), 180-184 (2008).

10. Pola J., Galikova A., Bastl Z., Vorlicek V., Bakardjieva S., Subrt J., Ouchi A.: UV Laser Photolysis of 1,3-Butadiyne and Formation of a Polyoxocarbosilane-Doped Nanosized Carbon. J. Photochem. Photobiol., A 194(2-3), 200-205 (2008).

11. Pola J., Marysko M., Vorlicek V., Bakardjieva S., Subrt J., Bastl Z., Ouchi A.: UV Laser Photolytic Solution Deposition of alpha-Fe/Polyoxocarbosilane/Carbon Nanocomposite and Evolution to alpha-Fe2O3/Polyoxocarbosilane/Carbon Nanocomposite. J. Photochem. Photobiol., A 199(2-3), 156-164 (2008).

12. Pola J., Ouchi A., Bakardjieva S., Vorlicek V., Marysko M., Subrt J., Bastl Z.: Laser Photochemical Etching of Silica: Nanodomains of Crystalline Chaoite and Silica in Amorphous C/Si/O/N Phase. J. Phys. Chem. C 112(34), 13281-13286 (2008).

13. Pola J., Pokorna D., Subrt J., Papagiannakopoulos P.: IR Laser-Induced Co-Decomposition of Gaseous Trisilane and Carbon Disulfide. J. Anal. Appl. Pyrolysis 81(2), 231-236 (2008).

14. Pola J., Urbanova M., Santos M., Diaz L., Subrt J.: IR Laser-Induced Co-Decomposition of Trisilane and Thiirane for Deposition of Polycarbosilthiane Films. J. Anal. Appl. Pyrolysis 81(2), 225-230 (2008).

15. Posta M., Cermak Jan, Sykora J., Vojtisek P., Cisarova I., Fajgar R.: Square-Planar Diphosphinoazine Rhodium(I) Amido Carbonyl Complexes with an Unsymmetrical PNP’ Pincer-type Coordination. J. Organomet. Chem. 693(11), 1997-2003 (2008).

16. Urbanova M., Pokorna D., Bakardjieva S., Subrt J., Bastl Z., Pola J.: IR Laser-Induced Carbothermal Reduction of Silica. Eur. J. Inorg. Chem. 2008(26), 4111-4116 (2008).

17. Blazevska-Gilev J., Bastl Z., Subrt J., Stopka P., Pola J.: IR Laser Ablative Degradation of Poly(phenylene ether sulfone): Deposition of Films Containing Sulfone, Sulfoxide and Sulfide Groups. Polym. Degrad. Stabil. 94(2), 196-200 (2009).

18. Drinek V., Vacek K.: IR Evidence of Peroxy Radical SiOO(.). Appl. Phys. A: Solids Surf., submitted.

International conferences

19. Blazevska-Gilev J., Pola J.: IR Laser Ablation of Poly(acetate) Loaded with Metal Particles. 20th Congress of Chemists and Technologists of Macedonia, Abstract Book, p. 268, Ohrid, Macedonia, 17-20 September 2008.

20. Blazevska-Gilev J., Pola J.: IR Laser Ablation of Poly(vinyl chloride-co vinyl acetate). 20th Congress of Chemists and Technologists of Macedonia, Abstract Book, p. 270, Ohrid, Macedonia, 17-20 September 2008.

21. Drinek V., Fajgar R., Klementova M., Subrt J.: From Shelled Germanium Nanowires to SiC Nanotubes. 6th International Conference on Inorganic Materials, Poster Presentations, Dresden, Germany, 28-30 September 2008.

22. Galikova A., Pola J.: TGA: A Sensitive Diagnosis of Thermal Stability of Laser-Deposited Materials. 35th International Conference of Slovak Society of Chemical Engineering, Proceedings, p. 153 (10 pp. full text on CD-ROM), Tatranske Matliare, Slovakia, 26-30 May 2008.

23. Klementova M., Drinek V., Fajgar R., Subrt J.: Structure of Coated Ge-nanowires. Microscopy and Microanalysis 2008, Book of Abstracts, Albuquerque, New Mexico, USA, 03-07 August 2008.

24. Tomovska R., Pola J.: ArF Laser Photolytic Deposition of Nanopolymeric Organosulfur Materials. 20th Congress of Chemists and Technologists of Macedonia , Abstract Book, pp. 57-58, Ohrid, Macedonia, 17-20 September 2008.

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