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Beam-induced crystallization of amorphous Me-Si-C (Me = Nb or Zr) thin films during transmission electron microscopy
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Inorganic Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Inorganic Chemistry.
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2013 (English)In: MRS Communications, ISSN 2159-6859, Vol. 3, no 3, 151-155 p.Article in journal (Refereed) Published
Abstract [en]

We report that an electron beam focused for high-resolution imaging rapidly initiates observable crystallization of amorphous Me-Si-C films. For 200-keV electron irradiation of Nb-Si-C and Zr-Si-C films, crystallization is observed at doses of similar to 2.8 x 10(9) and similar to 4.7 x 10(9) e(-)/nm(2), respectively. The crystallization process is driven by atomic displacement events, rather than heating from the electron beam as in situ annealing (400-600 degrees C) retains the amorphous state. Our findings demand a critical analysis of alleged amorphous and nanocrystalline ceramics including reassessing previous reports on nanocrystalline Me-Si-C films for possible electron-beam-induced crystallization effects.

Place, publisher, year, edition, pages
2013. Vol. 3, no 3, 151-155 p.
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:uu:diva-210740DOI: 10.1557/mrc.2013.31ISI: 000325095100007OAI: oai:DiVA.org:uu-210740DiVA: diva2:664273
Available from: 2013-11-14 Created: 2013-11-14 Last updated: 2015-07-07Bibliographically approved
In thesis
1. Synthesis and Characterization of Multifunctional Carbide- and Boride-based Thin Films
Open this publication in new window or tab >>Synthesis and Characterization of Multifunctional Carbide- and Boride-based Thin Films
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis present research on synthesis, microstructure, and properties of carbide- and boride- based thin films. The films have been synthesized by dc magnetron sputtering, and their microstructures have been characterized mainly by X-ray photoelectron spectroscopy (XPS), X-ray diffraction, and transmission electron microscopy.  One of the main objectives with this research has been to evaluate the thin films potential as materials for sliding electrical contact applications and this have influenced, which properties that have been evaluated.

Co-sputtered Nb-C films have a microstructure comprising of nanocrystalline NbCx  (nc-NbCx) grains embedded in a matrix of amorphous C (a-C). A thinner a-C matrix form in the Nb-C films compared to the well-studied Ti-C system. As a consequence, the Nb-C films have a higher hardness and conductivity than previously studied Ti-C sputtered under similar conditions. The promising electrical contact properties are attained for reactively sputtered Nb-C films under industrial conditions, at deposition rates two orders of magnitude higher. A reduction in crystallinity is seen when Si is added to the Nb-C films and amorphous films forms at Si content > 25 at.%. The alloying of Si was however not beneficial for the electrical contact properties.

Substoichiometric CrB2-x (B/Cr = 1.5) and NbB2-x (B/Nb = 1.8) films are achieved when deposited from MeB2 targets. Boron segregates to grain boundaries forming a B-rich tissue phase. This result in superhardness for the NbB2-x films (42 ± 4 GPa) as well as a low friction attributed to the formation of a boric acid film. Carbon forms a solid solution in the MeB2 grains as well as segregating to grain boundaries forming an amorphous BCx (a-BCx) phase when alloyed to CrB2-x and NbB2-x films. The formation of the a-BCx phase drastically improves the electrical contact resistance of the NbB2-x films. However, the mechanical properties are degraded, which result in a high friction and wear rate.

It was in TEM studies of the metastable amorphous structures for the Nb-Si-C films found that the electron beam induces crystallization. Hence, great care is required when studying these types of metastable structures.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2014. 79 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1127
Keyword
thin film, coating, magnetron sputtering, nanocomposite, boride, carbide, electrical properties, mechanical properties
National Category
Materials Chemistry
Research subject
Chemistry with specialization in Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-219040 (URN)978-91-554-8886-4 (ISBN)
Public defence
2014-04-04, Polhemssalen, Ångströmslaboratoriet, Lägerhyddsvägen 1, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2014-03-13 Created: 2014-02-20 Last updated: 2014-04-29
2. Synthesis and Characterization of Amorphous Carbide-based Thin Films
Open this publication in new window or tab >>Synthesis and Characterization of Amorphous Carbide-based Thin Films
2015 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this thesis, research on synthesis, structure and characterization of amorphous carbide-based thin films is presented. Crystalline and nanocomposite carbide films can exhibit properties such as high electrical conductivity, high hardness and low friction and wear. These properties are in many cases structure-related, and thus, within this thesis a special focus is put on how the amorphous structure influences the material properties.

Thin films within the Zr-Si-C and Cr-C-based systems have been synthesized by magnetron sputtering from elemental targets. For the Zr-Si-C system, completely amorphous films were obtained for silicon contents of 20 at.% or higher. Modeling of these films, as well as experimental results suggest that the films exhibit a network-type structure where the bond types influence the material properties. Higher hardness and resistivity were observed with high amounts of covalent Si-C bonds.

Several studies were performed in the Cr-C-based systems. Cr-C films deposited in a wide composition range and with substrate temperatures of up to 500 °C were found to be amorphous nanocomposites, consisting of amorphous chromium carbide (a-CrCx) and amorphous carbon (a-C) phases. The carbon content in the carbidic phase was determined to about 30-35 at.% for most films. The properties of the Cr-C films were very dependent of the amount of a-C phase, and both hardness and electrical resistivity decreased with increasing a-C contents. However, electrochemical analysis showed that Cr-C films deposited at higher substrate temperature and with high carbon content exhibited very high oxidation resistance. In addition, nanocomposite films containing Ag nanoparticles within an amorphous Cr-C matrix were studied in an attempt to improve the tribological properties. No such improvements were observed but the films exhibited a better contact resistance than the corresponding binary Cr-C films. Furthermore, electrochemical analyses showed that Ag nanoparticles on the surface affected the formation of a stable passive film, which would make the Cr-C/Ag films less resilient to oxidation than the pure Cr-C films.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2015. 63 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1239
Keyword
Amorphous, coating, thin film, nanocomposite, sputter deposition, PVD, XPS, SEM, TEM, electrical properties, mechanical properties
National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-247282 (URN)978-91-554-9198-7 (ISBN)
Public defence
2015-05-08, Häggsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:15 (English)
Opponent
Supervisors
Available from: 2015-04-16 Created: 2015-03-16 Last updated: 2015-07-07

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Nedfors, NilsAndersson, MatildaJansson, Ulf

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