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Carbide and MAX-Phase Engineering by Thin Film Synthesis Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology 930 Carbide and MAX-Phase Engineering by Thin Film Synthesis JENS-PETTER PALMQUIST ACTA UNIVERSITATIS UPSALIENSIS UPPSALA 2004 ! ""# $%&$' ( ( ( ) * + , ) - ./) ""#) 0 123/ , * 4 ) 56 123/( ( 7) 2 ) 8%") !" ) ) 94:; 8$/''#/'<'</" * ( +/ ( 123/ ( + ) 1 ( ( - ( ( ) ( = = 0 >/=0$/ ( + ( + =- 0 + $"" 0) = ( + " ? 0 / (( + ( %' @ ) ( ( *$/A0 ( ( / /( ( + ( () 1 + 5;1 70 5*=70 () * ( 40 / + ) 2 ( ( ( 123/ ) * ( ( + 1 B$23 C$ % + 1 2 $%/$# 30 ;) * + ( ( - ( ) 4 ( 123/ / D ( ) E + ( ( 123/ ( + !'" 0) ( / ( ( *%40 *%20 * 20 + ) * + 123/ *#40%) 9 + + 123/ *'4 0% *!4 0') 0 + ( + + D ) ( 123/ ( + ( ( ( +/( + ) * ( =0 123/ *%40 0 A F 4 1 F41 !" "# $ % $ &' ()*$ $ +!,(-.- $ G . / - ""# 944; $$"#/ % 3 94:; 8$/''#/'<'</" & &&& /%8! 5 &HH )D)H I C & &&& /%8! 7 Printed in Sweden by Universitetstryckeriet, Uppsala 2004 Till Professor Baltazar Carbide and MAX-Phase Engieneering by Thin Film Synthesis List of publications This thesis is based on the following publications, chronologically numbered and referred to in the text by their Roman numerals. I. Deposition of epitaxial ternary transition metal carbide films. J.-P. Palmquist, J. Birch, U. Jansson, Thin Solid Films 405 (2002) p. 122. II. Magnetron sputtered W-C films with C60 as carbon source. J.-P. Palmquist, Zs. Czigany, M. Odén, J. Neidhart, L. Hultman, U. Jansson, Thin Solid Films 444 (2003) p. 29. III. Epitaxial growth of tungsten carbide films using C60 as carbon precursor. J.-P. Palmquist, Zs. Czigany, L. Hultman, U. Jansson, Journal of Crystal Growth 259 (2003) p. 12. IV. Magnetron sputtered epitaxial single-phase Ti3SiC2 thin films. J.-P. Palmquist, U. Jansson, T. Seppänen, P. O. Å. Persson, J. Birch, L. Hultman, P. Isberg, Applied Physics Letters 81 (2002) p. 835. V. Kink formation around indents in laminated Ti3SiC2 thin films studied in the nanoscale. J. M. Molina-Aldareguia, J. Emmerlich, J.-P. Palmquist, U. Jansson, L. Hultman, Scripta Materialia 49 (2003) p. 155. VI. New MAX phases in the Ti-Si-C system studied by thin film synthesis and ab initio calculations. J.-P. Palmquist, S. Li, P. O. Å. Persson, J. Emmerlich, O. Wilhelmsson, H. Högberg, M. I. Katsnelson, B. Johansson, R. Ahuja, O. Eriksson, L. Hultman, U. Jansson, Submitted to: Physical Review B (2003). VII. Growth of Ti3SiC2 thin films by elemental target magnetron sputtering. J. Emmerlich, J.-P. Palmquist, H. Högberg, Zs. Czigány, Sz. Sasvàri, P. O. Å. Persson, U. Jansson, L. Hultman, In manuscript (2004). VIII. Sputtering of Ti2AlC and Ti3AlC2 thin films. O. Wilhelmsson, J.-P. Palmquist, T. Nyberg, U. Jansson, Submitted to: Applied Physical Letters (2004). IX. Electronic structure of the MAX-phases Ti3AC2 (A=Al, Si, Ge) investigated by soft x-ray absorption and emission spectroscopies. M. Magnuson, J.-P. Palmquist, S. Li, M. Mattesini, R. Ahuja, O. Eriksson, O. Wilhelmsson, P. Eklund, H. Högberg, L. Hultman, U. Jansson, In manuscript (2004). Uppsala University i Carbide and MAX-Phase Engieneering by Thin Film Synthesis Publications not included in this thesis: X. The formation and characterization of epitaxial titanium carbide contacts to 4H-SiC. S.-K. Lee, E. Danielsson, C.-M. Zetterling, M. Ostling, J.-P. Palmquist, H. Hogberg, U. Jansson, Materials Research Society Symposium - Proceedings 622 (2000) T691. XI. Electrical characterization of TiC ohmic contacts to aluminum ion implanted 4H-silicon carbide. S.-K. Lee, C.-M. Zetterling, E. Danielsson, M. Ostling, J.-P. Palmquist, H. Hogberg, U. Jansson, Applied Physics Letters 77 (2000) p. 1478. XII. Low resistivity ohmic titanium carbide contacts to n- and p-type 4H- silicon carbide. S.-K. Lee, C.-M. Zetterling, M. Ostling, J.-P. Palmquist, H. Hogberg, U. Jansson Solid-State Electronics 44 (2000) p. 1179. XIII. Low temperature epitaxial growth of metal carbides using fullerenes. U. Jansson, H. Hogberg, J.-P. Palmqvist, L. Norin, J. O. Malm, L. Hultman, J. Birch Surface and Coatings Technology 142-144 (2001) p. 817. XIV. Low resistivity ohmic contacts on 4H-silicon carbide for high power and high temperature device applications. S.-K. Lee, C.-M. Zetterling, M. Ostling, J.-P. Palmquist, U. Jansson, Microelectronic Engineering 60 (2002) p. 261. XV. Structural characterization of epitaxial Ti3SiC2 films. T. Seppänen, J.-P. Palmquist, P. O. Å. Persson, J. Emmerlich, J. Molina, J. Birch, U. Jansson, P. Isberg, L. Hultman, Conference Proceeding: the 53rd annual Meeting of The Scandinavian Society for Electron Microscopy (SCANDEM), ISSN 1455-4518, Tampere, Finland, (2002), p. 142 XVI. Growth and characterization of MAX-phase thin films. H. Högberg, L. Hultman, J. Emmerlich, T. Joelsson, P. Eklund, J. M. Molina- Aldareguia, J.-P. Palmquist, O. Wilhelmsson, U. Jansson, Conference Proceedings: The 4th Asian-European International Conference on Plasma Surface Engineering (AEPSE), Jeju, Korea, (2003). (To be published in Thin Solid Film or Surface and Coatings Technology.) Also not included in this thesis is the following patent. XVII. Method of synthesising a compound of the formula Mn+1AXn, film of the compound and its use. J.-P. Palmquist, U. Jansson, J. Birch, L. Hultman, P. Isberg, T. Seppänen, International publication number: WO03046247 (5 June 2003). ii Jens-Petter Palmquist Carbide and MAX-Phase Engieneering by Thin Film Synthesis Comments on my participation In the papers and manuscripts that I am first author, Publication I,-IV and VI, I have performed the experimental work, most of the characterisation and written the major part of the manuscripts. In the deformation study in Publication V, I have deposited the films and taken part in planning and discussion. In Publication VI, I have taken part in planning and discussion of the theoretical study, but not performed the calculations. In Publication VII and VIII, I have taken part in planning, experimental work and some characterisation and contributed to the discussion of writing. Publication IX is a soft x-ray study on the MAX-phase films where I have made some of the films and taken part in the discussion and writing. Publication X-XVI, are mentioned since I have been part of the thin film depositions and also performed some characterisation. They also deal with an important possible application of epitaxial carbides as a contact material in SiC- based microelectronics. All electron microscopy studies are made in cooperation with the Thin Film Physics Group, IFM at Linköping University. The co-authors are greatly acknowledged for the opportunity I have had to work with you. Uppsala University iii Carbide and MAX-Phase Engieneering by Thin Film Synthesis Contents List of publications.....................................................................................................i Comments on my participation................................................................... iii Chapter 1. Introduction .....................................................................................1 1.1 Motivation and background .........................................................1 1.2 Materials engineering...................................................................2 Chapter 2. Carbides and MAX-phases.............................................................4 2.1 Transition metal carbides.............................................................4 2.2 The Mn+1AXn phases....................................................................6 Chapter 3. Thin films .........................................................................................9 3.1 Synthesis techniques ....................................................................9 3.1.1 Evaporation .............................................................................9 3.1.2 Sputtering..............................................................................10 3.2 Film growth................................................................................11 3.2.1 Epitaxial growth....................................................................12 3.2.2 Pseudomorphic growth..........................................................14 Chapter 4. Characterisation ............................................................................16 4.1 X-ray diffraction ........................................................................16 4.1.1 Thin film diffraction..............................................................16 4.1.2 Reciprocal space mapping (RSM).........................................18 4.2 Transmission electron microscopy.............................................19 4.3 X-ray photoelectron spectroscopy .............................................20 4.4 Four point probe measurements.................................................21 4.5 Nanoindentation.........................................................................22 4.6 Soft x-ray spectroscopy..............................................................22 Chapter
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