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Synthesis and Characterization of New MAX Phase Alloys
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This Thesis explores synthesis and characterization of new MAX phase alloys (M = early transition metal, A = A-group element, and X = C or N), based on incorporation of M and X elements previously not considered. My primary focus is on M = Mn for attaining magnetic properties, and on X = O for potential tuning of the transport properties. A recent theoretical study predicted (Cr1-xMnx)2AlC MAX phase to be a stable magnetic nanolaminate. I aimed at realizing this material and through a combinatorial approach based on magnetron sputtering from elemental targets, the first experimental evidence of Mn incorporation (x = 0.16) in a MAX phase is presented. The corresponding MAX phase was also synthesized using cathodic arc film deposition (x = 0.20) and bulk synthesis methods (x = 0.06). The primary characterization techniques were X-ray diffraction and high-resolution (scanning) transmission electron microscopy in combination with energy dispersive X-ray spectroscopy and/or electron energy loss spectroscopy, to obtain a precise local quantification of the MAX phase composition and to perform lattice resolved imaging. For epitaxial film growth of (Cr1-xMnx)2AlC, evidence is presented for the formation of (Cr1-yMny)5Al8, exhibiting a bcc structure with an interplanar spacing matching exactly half a unit cell of the hexagonal MAX phase. Consequently, routinely performed X-ray diffraction symmetric θ-2θ measurements result in peak positions that are identical for the two phases. As (Cr1-yMny)5Al8 is shown to display a magnetic response, its presence needs to be taken into consideration when evaluating the magnetic properties of the MAX phase. Methods  to distinguish between (Cr1-yMny)5Al8 and (Cr1-xMnx)2AlC are also suggested. As different A-element in the MAX phase is theoretically predicted to influence phase stability, attainable level of Mn  incorporation, as well as magnetic properties, thin films of (Cr0.75Mn0.25)2GeC and bulk (Cr0.7Mn0.3)2GaC have also been synthesized. Vibrating sample magnetometry measurements display a magnetic response for all these materials, identifying (Cr,Mn)2AlC, (Cr,Mn)2GeC, and (Cr,Mn)2GaC as the first magnetic MAX phases. The results presented in this Thesis show that A = Al displays the highest magnetic transition temperature (well above room temperature) and A = Ga allows the highest Mn content. The attainable O incorporation in Ti2Al(C1-xOx)MAX phase was explored by arc deposition of Ti2AlC1-y thin films under high vacuum conditions, and solid-state reactions following deposition of understoichiometric TiCz on Al2O3. Ti2Al(C1-xOx)thin films with up to 13 at.% O (x = 0.52) were synthesized, and O was shown to occupy the C lattice site. The obtained O concentration is enough to allow future experimental investigations of the previously suggested (from theory) substantial change in anisotropic electronic properties with increasing O content. The experimental results obtained in this Thesis expand the MAX phase definition and the materials characteristics into new research areas, towards further fundamental understanding and functionalization.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2014. , 58 p.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1573
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-104829DOI: 10.3384/diss.diva-104829ISBN: 978-91-7519-407-3 (print)OAI: oai:DiVA.org:liu-104829DiVA: diva2:699502
Public defence
2014-03-20, Planck, Fysikhuset, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2014-02-27 Created: 2014-02-27 Last updated: 2016-12-28Bibliographically approved
List of papers
1. Synthesis and ab initio calculations of nanolaminated (Cr,Mn)2AlC compounds
Open this publication in new window or tab >>Synthesis and ab initio calculations of nanolaminated (Cr,Mn)2AlC compounds
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2013 (English)In: Physical Review B. Condensed Matter and Materials Physics, ISSN 1098-0121, E-ISSN 1550-235X, Vol. 87, no 9Article in journal (Refereed) Published
Abstract [en]

We present an ab initio theoretical analysis of the temperature-dependent stability of inherently nanolaminated (Cr1−xMnx)2AlC. The results indicate energetic stability over the composition range x = 0.0 to 0.5 for temperatures ≥600 K. Corresponding thin film compounds were grown by magnetron sputtering from four elemental targets. X-ray diffraction in combination with analytical transmission electron microscopy, including electron energy-loss spectroscopy and energy dispersive x-ray spectroscopy analysis, revealed that the films were epitaxial (0001)-oriented single-crystals with x up to 0.16.

Place, publisher, year, edition, pages
American Physical Society, 2013
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-91544 (URN)10.1103/PhysRevB.87.094113 (DOI)000316663700002 ()
Note

Funding Agencies|European Research Council under the European Community|258509227754|Knut and Alice Wallenberg Foundation||Swedish Research Council|||DFG-SPP 1299|

Available from: 2013-04-26 Created: 2013-04-26 Last updated: 2017-12-06
2. Magnetic Self-Organized Atomic Laminate from First Principles and Thin Film Synthesis
Open this publication in new window or tab >>Magnetic Self-Organized Atomic Laminate from First Principles and Thin Film Synthesis
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2013 (English)In: Physical Review Letters, ISSN 0031-9007, E-ISSN 1079-7114, Vol. 110Article in journal (Refereed) Published
Abstract [en]

he first experimental realization of a magnetic Mn+1AXn (MAX) phase, (Cr0.75Mn0.25)2GeC, is presented, synthesized as a heteroepitaxial single crystal thin film, exhibiting excellent structural quality. This self-organized atomic laminate is based on the well-known Cr2GeC, with Mn, a new element in MAX phase research, substituting Cr. The compound was predicted using first-principles calculations, from which a variety of magnetic behavior is envisaged, depending on the Mn concentration and Cr/Mn atomic configuration within the sublattice. The analyzed thin films display a magnetic signal at room temperature.

Place, publisher, year, edition, pages
American Physical Society, 2013
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-104824 (URN)10.1103/PhysRevLett.110.195502 (DOI)
Available from: 2014-02-27 Created: 2014-02-27 Last updated: 2017-12-05Bibliographically approved
3. Synthesis and characterization of arc deposited magnetic (Cr,Mn)2AlC MAX phase films
Open this publication in new window or tab >>Synthesis and characterization of arc deposited magnetic (Cr,Mn)2AlC MAX phase films
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2014 (English)In: Physica Status Solidi. Rapid Research Letters, ISSN 1862-6254, E-ISSN 1862-6270, Vol. 8, no 5, 420-423 p.Article in journal (Refereed) Published
Abstract [en]

(Cr1-xMnx)2AlC MAX phase thin films were synthesized by cathodic arc deposition. Scanning transmission electron microscopy including local energy dispersive X-ray spectroscopy analysis of the as-deposited films reveals a Mn incorporation of 10 at.% in the structure, corresponding to x = 0.2. Magnetic properties were characterized with vibrating sample magnetometry, revealing a magnetic response up to at least room temperature, thus verifying previous theoretical predictions of an antiferromagnetic or ferromagnetic ground state for Cr2AlC upon alloying with Mn.

Place, publisher, year, edition, pages
Wiley-Blackwell, 2014
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-96998 (URN)10.1002/pssr.201409087 (DOI)000336495000009 ()
Available from: 2013-09-02 Created: 2013-09-02 Last updated: 2017-12-06Bibliographically approved
4. Structural and magnetic properties of (Cr1-xMnx)(5)Al-8 solid solution and structural relation to hexagonal nanolaminates
Open this publication in new window or tab >>Structural and magnetic properties of (Cr1-xMnx)(5)Al-8 solid solution and structural relation to hexagonal nanolaminates
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2014 (English)In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 49, no 20, 7099-7104 p.Article in journal (Refereed) Published
Abstract [en]

Electron microscopy is used to reveal the competitive epitaxial growth of bcc structure (Cr1-x Mn (x) )(5)Al-8 and (Cr1-y Mn (y) )(2)AlC [M (n+1)AX (n) (MAX)] phase during both magnetron sputtering and arc deposition. X-ray diffraction theta-2 theta measurements display identical peak positions of (000n)-oriented MAX phase and (Cr1-x Mn (x) )(5)Al-8, due to the interplanar spacing of (Cr1-x Mn (x) )(5)Al-8 that matches exactly half a unit cell of (Cr1-y Mn (y) )(2)AlC. Vibrating sample magnetometry shows that a thin film exclusively consisting of (Cr1-x Mn (x) )(5)Al-8 exhibits a magnetic response, implying that the potential presence of this phase needs to be taken into consideration when evaluating the magnetic properties of (Cr, Mn)(2)AlC.

Place, publisher, year, edition, pages
Springer Verlag (Germany), 2014
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-109870 (URN)10.1007/s10853-014-8416-8 (DOI)000339963800028 ()
Note

Funding Agencies|European Research Council under the European Communities Seventh Framework Programme (FP7)/ERC [258509]; Swedish Research Council [642-2013-8020]; KAW Fellowship program; Swedish Research Council; Knut and Alice Wallenberg Foundation; SSF Synergy Grant FUNCASE Functional Carbides and Advanced Surface Engineering; Carl Trygger Foundation

Available from: 2014-08-28 Created: 2014-08-28 Last updated: 2017-12-05
5. Solid Solubility and Magnetism upon Mn Incorporation in the Bulk Ternary Carbides Cr2AlC and Cr2GaC
Open this publication in new window or tab >>Solid Solubility and Magnetism upon Mn Incorporation in the Bulk Ternary Carbides Cr2AlC and Cr2GaC
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2015 (English)In: Materials Research Letters, ISSN 2166-3831, Vol. 3, no 1, 16-22 p.Article in journal (Refereed) Published
Abstract [en]

Herein, we report on the bulk synthesis of (Cr1-xMnx)(2)AlC and (Cr1-yMny)(2)GaC MAX phases. Scanning electron and transmission electron microscopy, in combination with energy-dispersive X-ray spectroscopy performed locally on MAX phase grains, revealed x and y to be 0.06 (3 at%) and 0.3 (15 at%), respectively. The introduction of Mn into the structure did not result in appreciable changes in the c-lattice constants. Vibrating sample magnetometry measurements suggest that bulk (Cr0.7Mn0.3)(2)GaC may be magnetic.

Place, publisher, year, edition, pages
Taylor & Francis, 2015
Keyword
MAX Phases, Solid Solution, Bulk Synthesis, Magnetism
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-127069 (URN)10.1080/21663831.2014.944676 (DOI)000372215500003 ()
Note

At the time for thesis presentation publication was in status: Manuscript,

At the time for thesis presentation manuscript was named: Solid solubility and magnetism upon Mn incorporation in bulk Cr2AlC and Cr2GaC MAX phases

Funding Agencies|European Research Council under the European Communitys Seventh Framework Programme [258509]; Swedish Research Council (VR) [621-2012-4425, 642-2013-8020]; Knut and Alice Wallenberg (KAW) Academy Fellowship Program; SSF synergy grant FUNCASE Functional Carbides and Advanced Surface Engineering

Available from: 2016-04-13 Created: 2016-04-13 Last updated: 2016-12-28Bibliographically approved
6. Oxygen incorporation in Ti2AlC thin films studied by electron energy loss spectroscopy and ab initio calculations
Open this publication in new window or tab >>Oxygen incorporation in Ti2AlC thin films studied by electron energy loss spectroscopy and ab initio calculations
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2013 (English)In: Journal of Materials Science, ISSN 0022-2461, E-ISSN 1573-4803, Vol. 48, no 10, 3686-3691 p.Article in journal (Refereed) Published
Abstract [en]

Substitution of C with O in hexagonal inherently nanolaminated Ti2AlC has been studied experimentally and theoretically. Ti2Al(C1−x O x ) thin films with x ≤ 0.52 are synthesized by both cathodic arc deposition with the uptake of residual gas O, and solid-state reaction between understoichiometric TiC y and Al2O3(0001) substrates. The compositional analysis is made by analytical transmission electron microscopy, including electron energy loss spectroscopy. Furthermore, predictive ab initio calculations are performed to evaluate the influence of substitutional O on the shear stress at different strains for slip on the (0001) basal plane in the [−1010] and [1−210] directions.

Place, publisher, year, edition, pages
Springer Verlag (Germany), 2013
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-90742 (URN)10.1007/s10853-013-7165-4 (DOI)000315518400009 ()
Note

Funding Agencies|European Research Council under the European Community|258509227754|Swedish Research Council (VR)||

On the day of the defence date of the Licentiate Thesis, the status of this article was Manuscript.

Available from: 2013-04-19 Created: 2013-04-05 Last updated: 2017-12-06Bibliographically approved

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