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ZrB2 Thin Films: Growth and Characterization
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, Faculty of Science & Engineering.
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Zirconium diboride, ZrB2, is a ceramic material with bulk properties such as high melting point (3245 °C), high hardness (23 GPa), and low resistivity (~8 μΩcm). Thin film growth of ZrB2 using physical vapor deposition has suffered from problems with films deviating from stoichiometry and with high levels of contaminants, especially high oxygen content. The homogeneity range of ZrB2 is very narrow, and consequently it is vital to achieve the correct stoichiometry to grow films with high crystalline order.

This thesis describes a direct current magnetron sputtering process to grow stoichiometric ZrB2 thin films with a low degree of impurities. Growth of epitaxial ZrB2 films was achieved on 4H-SiC(0001), Si(111) and Al2O3(0001) substrates. The effect of deposition temperature and power applied on the sputtering target was investigated and showed that high power density (8.77 Wcm-2) and high temperature (900 °C) resulted in films with the best composition and the highest crystal quality. ZrB2 films on GaN(0001) templates exhibit an amorphous layer at the film-substrate interface and the resulting films are either polycrystalline or textured.

Resistivity measurements showed that the ZrB2 thin films exhibit typical resistivity values of ~100-250 μΩcm and that the resistivity decreased with increasing deposition temperature.

Nanoindentation was applied to assess the mechanical properties of the films. The epitaxial ZrB2 films exhibit high elastic recovery and a hardness of ~45-50 GPa, twice as high as the literature bulk value. In addition, evaluation of the mechanical properties was performed at high temperatures of up to 600 °C and showed that the epitaxial films retained a higher hardness, compared to textured ZrB2 films and bulk, also at these temperatures.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2016. , 67 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1744
National Category
Physical Sciences
Identifiers
URN: urn:nbn:se:liu:diva-128614DOI: 10.3384/diss.diva-128614ISBN: 978-91-7685-833-2 (print)OAI: oai:DiVA.org:liu-128614DiVA: diva2:930718
Public defence
2016-06-17, Planck, Fysikhuset, Campus Valla, Linköping, 09:15 (English)
Opponent
Supervisors
Available from: 2016-05-25 Created: 2016-05-25 Last updated: 2016-08-31Bibliographically approved
List of papers
1. Direct current magnetron sputtered ZrB2 thin films on 4H-SiC(0001) and Si(100)
Open this publication in new window or tab >>Direct current magnetron sputtered ZrB2 thin films on 4H-SiC(0001) and Si(100)
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2014 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 550, 285-290 p.Article in journal (Other academic) Published
Abstract [en]

ZrB2 thin films have been synthesized using direct current magnetron sputtering from a ZrB2 compound target onto 4H-SiC(0001) and Si(100) substrates kept at different temperatures (no heating, 400 °C, and 550 °C), and substrate bias voltage (-20 V to -80 V). Time-of-flight energy elastic recoil detection analysis shows that all the films are near stoichiometric and have a low degree of contaminants, with O being the most abundant (< 1 at.%). The films are crystalline, and their crystallographic orientation changes from 0001 to a more random orientation with increased deposition temperature. X-ray diffraction pole figures and selected area electron diffraction patterns of the films deposited without heating reveal a fiber-texture growth. Four point probe measurements show typical resistivity values of the films ranging from ~95 to 200 μΩcm, decreasing with increased growth temperature and substrate bias.

Keyword
Zirconium diboride; Silicon carbide; Thin films; Compound target; Industrial scale deposition system; Crystalline films
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-99942 (URN)10.1016/j.tsf.2013.11.040 (DOI)000328499700045 ()
Available from: 2013-10-23 Created: 2013-10-23 Last updated: 2017-12-06Bibliographically approved
2. Magnetron sputtering of epitaxial ZrB2 thin films on 4H-SiC(0001) and Si(111)
Open this publication in new window or tab >>Magnetron sputtering of epitaxial ZrB2 thin films on 4H-SiC(0001) and Si(111)
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2014 (English)In: Physica Status Solidi (a), ISSN 1862-6319, Vol. 211, no 3, 636-640 p.Article in journal (Refereed) Published
Abstract [en]

Epitaxial ZrB2 thin films were deposited at a temperature of 900 °C on 4H-SiC(0001) and Si(111) substrates by magnetron sputtering from a ZrB2 source at high rate ~80 nm/min. The films were analyzed by thin film X-ray diffraction including pole figure measurements and reciprocal space mapping as well as high resolution electron microscopy.

Place, publisher, year, edition, pages
John Wiley & Sons, 2014
Keyword
Zirconium diboride Epitaxial growth Silicon carbide Thin films Magnetron sputtering
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-99944 (URN)10.1002/pssa.201330308 (DOI)000333194100018 ()
Available from: 2013-10-23 Created: 2013-10-23 Last updated: 2016-08-31Bibliographically approved
3. Stoichiometric, epitaxial ZrB2 thin films with low oxygen-content deposited by magnetron sputtering from a compound target: Effects of deposition temperature and sputtering power
Open this publication in new window or tab >>Stoichiometric, epitaxial ZrB2 thin films with low oxygen-content deposited by magnetron sputtering from a compound target: Effects of deposition temperature and sputtering power
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2015 (English)In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 430, 55-62 p.Article in journal (Refereed) Published
Abstract [en]

Zirconium diboride (ZrB2) thin films have been deposited on 4H-SiC(0001) substrates by direct current magnetron sputtering from a compound target. The effect of deposition temperature (500-900 degrees C) and sputtering power (100-400 W) on the composition and structure of the films have been investigated. Electron microscopy and X-ray diffraction reveal that high sputtering power values and high deposition temperatures are favorable to enhance the crystalline order of the epitaxial 0001 oriented films. X-ray photoelectron spectroscopy shows that the composition of the films is near-stoichiometric for all deposition temperatures and for high sputtering power values of 300 W and 400 W, whereas under-stoichiometric films arc obtained when applying 100 W or 200 W. Decreasing the deposition temperature, or in particular the sputtering power, result in higher C and O impurity levels. The resistivity of the films was evaluated by four-point-probe measurements and found to scale with the amount of O impurities in the films. The lowest resistivity value obtained is 130 mu Omega cm, which makes the ZrB2 films interesting as an electrical contact material. (C) 2015 Elsevier B.V. All rights reserved.

Place, publisher, year, edition, pages
ELSEVIER SCIENCE BV, 2015
Keyword
X-ray diffraction; X-ray photoelectron spectroscopy; Physical vapor deposition processes; Borides
National Category
Physical Sciences Chemical Sciences
Identifiers
urn:nbn:se:liu:diva-122186 (URN)10.1016/j.jcrysgro.2015.08.012 (DOI)000362014800010 ()
Note

Funding Agencies|Swedish Research Council (VR) [621 2010-3921]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University (Faculty Grant) [SFO-Mat-LiU 2009-00971]; VINN Excellence Center Functional Nanoscale Materials (FunMat) [2005-02666]; Knut and Alice Wallenberg Foundation [2011.0143]

Available from: 2015-10-26 Created: 2015-10-23 Last updated: 2017-12-01
4. Hard and elastic epitaxial ZrB2 thin films on Al2O3(0001) substrates deposited by magnetron sputtering from a ZrB2 compound target
Open this publication in new window or tab >>Hard and elastic epitaxial ZrB2 thin films on Al2O3(0001) substrates deposited by magnetron sputtering from a ZrB2 compound target
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2016 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 111, 166-172 p.Article in journal (Refereed) Published
Abstract [en]

Zirconium diboride (ZrB2) exhibits high hardness and high melting point, which is beneficial for applications in for e.g. metal cutting. However, there is limited data on the mechanical properties of ZrB2 films and no data on epitaxial films. In this study, ZrB2(0001) thin films, with thicknesses up to 1.2 μm, have been deposited on Al2O3(0001) substrates by direct current magnetron sputtering from a compound target. X-ray diffraction and transmission electron microscopy show that the films grow epitaxially with two domain types exhibiting different in-plane epitaxial relationships to the substrate. The out-of-plane epitaxial relationship was determined to ZrB2(0001)|Al2O3(0001) and the in-plane relationships of the two domains to ZrB2[100]‖Al2O3[100] and ZrB2[110]‖Al2O3[100]. Mechanical properties of the films, evaluated by nanoindentation, showed that all films exhibit hardness values above 45 GPa, a reduced Young's modulus in the range 350–400 GPa, and a high elastic recovery of 70% at an applied load of 9000 μN.

Place, publisher, year, edition, pages
Elsevier, 2016
Keyword
Borides, Epitaxial growth, Mechanical properties, Nanoindentation, Sputter deposition
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-128612 (URN)10.1016/j.actamat.2016.03.064 (DOI)000375812100018 ()
Note

Funding agencies: Swedish Research Council (VR) [621-2010-3921]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University [2009-00971]; Knut and Alice Wallenberg Foundation

Available from: 2016-05-25 Created: 2016-05-25 Last updated: 2017-11-30Bibliographically approved
5. High-temperature nanoindentation of epitaxial ZrB2 thin films
Open this publication in new window or tab >>High-temperature nanoindentation of epitaxial ZrB2 thin films
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2016 (English)In: Scripta Materialia, ISSN 1359-6462, E-ISSN 1872-8456, Vol. 124, 117-120 p.Article in journal (Refereed) Published
Abstract [en]

We use in-situ heated nanoindentation to investigate the high-temperature nanomechanical properties of epitaxial and textured ZrB2 films deposited by magnetron sputtering. Epitaxial films deposited on 4H-SiC(0001) show a hardness decrease from 47 GPa at room temperature to 33 GPa at 600 °C, while the reduced elastic modulus does not change significantly. High resolution electron microscopy (HRTEM) with selected area electron diffraction of the indented area in a 0001-textured film reveals a retained continuous ZrB2 film and no sign of crystalline phase transformation, despite massive deformation of the Si substrate. HRTEM analysis supports the high elastic recovery of 96% in the films.

Place, publisher, year, edition, pages
Elsevier, 2016
Keyword
Sputtering; Borides; Ceramic thin film; Nanoindentation; Transmission electron microscopy
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-130917 (URN)10.1016/j.scriptamat.2016.06.033 (DOI)000383294200027 ()
Note

Funding agencies: Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University (Faculty Grant SFO-Mat-LiU) [2009-00971]; Swedish Research Council (VR) [621-2010-3921]

Available from: 2016-08-31 Created: 2016-08-31 Last updated: 2017-11-21Bibliographically approved
6. ZrB2 thin films deposited on GaN(0001) by magnetron sputtering from a ZrB2 target
Open this publication in new window or tab >>ZrB2 thin films deposited on GaN(0001) by magnetron sputtering from a ZrB2 target
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2016 (English)In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 453, 71-76 p.Article in journal (Refereed) Published
Abstract [en]

ZrB2 films were deposited on 900 °C-preheated or non-preheated GaN(0001) surfaces by direct current magnetron sputtering from a compound target. Analytical transmission electron microscopy and scanning transmission electron microscopy with energy dispersive X-ray spectroscopy and electron energy loss spectroscopy revealed a 0001 fiber textured ZrB2 film growth following the formation of a ~2 nm thick amorphous BN layer onto the GaN(0001) at a substrate temperature of 900 °C. The amorphous BN layer remains when the substrate temperature is lowered to 500 °C or when the preheating step is removed from the process and results in the growth of polycrystalline ZrB2 films. The ZrB2 growth phenomena on GaN(0001) is compared to on 4H-SiC(0001), Si(111), and Al2O3(0001) substrates, which yield epitaxial film growth. The decomposition of the GaN surface during vacuum processing during BN interfacial layer formation is found to impede epitaxial growth of ZrB2.

Place, publisher, year, edition, pages
Elsevier, 2016
Keyword
A1. X-ray diffraction; A1. Interfaces; A1. Energy-dispersive X-ray spectroscopy; A1. Electron energy loss spectroscopy; A3. Physical vapor deposition processes; B1. Borides
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-130920 (URN)10.1016/j.jcrysgro.2016.08.011 (DOI)000386984000012 ()
Available from: 2016-08-31 Created: 2016-08-31 Last updated: 2017-11-21Bibliographically approved

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