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Multifunctional nanostructured Ti-Si-C thin films
Linköping University, Department of Physics, Chemistry and Biology, Thin Film Physics. Linköping University, The Institute of Technology.ORCID iD: 0000-0003-1785-0864
2007 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this Thesis, I have investigated multifunctional nanostructured Ti-Si-C thin films synthesized by magnetron sputtering in the substrate-temperature range from room temperature to 900 °C. The studies cover high-temperature growth of Ti3SiC2 and Ti4SiC3, low-temperature growth of Ti-Si-C nanocomposites, and Ti-Si-C-based multi¬layers, as well as their electrical, mechanical, and thermal-stability properties. Ti3SiC2 and Ti4SiC3 were synthesized homoepitaxially onto bulk Ti3SiC2 from individual sputtering targets and heteroepitaxially onto Al2O3(0001) substrates from a Ti3SiC2 target at substrate temperatures of 700 – 900 °C. In the latter case, the film composition exhibits excess C compared to the nominal target composition due to differences between species in angular and energy distribution and gas-phase scattering processes. Ti buffering is shown to compensate for this excess C. The electrical-resistivity values of Ti3SiC2 and Ti4SiC3 thin films were measured to 21-32 uOhmcm and ~50 uOhmcm, respectively. The good conductivity is because the presence of Si layers enhances the relative strength of the metallic Ti-Ti bonds. The higher density of Si layers in Ti3SiC2 than in Ti4SiC3 explains why Ti3SiC2 is the better conductor of the two. Ti3SiC2 thin films are shown to be thermally stable up to 1000 – 1100 °C. Annealing at higher temperature results in decomposition of Ti3SiC2 by Si out-diffusion to the surface with subsequent evaporation. Above 1200 °C, TiCx layers recrystallized. Nanocomposites comprising nanocrystalline (nc-)TiC in an amorphous (a-)SiC matrix phase were deposited at substrate temperatures in the range 100 – 300 °C. These nc-TiC/a-SiC films exhibit low contact resistance in electrical contacts and a ductile deformation behavior due to rotation and gliding of nc-TiC grains in the matrix. The ductile mechanical properties of nc-TiC/a-SiC are actually more similar to those of Ti3SiC2, which is very ductile due to kinking and delamination, than to those of the brittle TiC. Epitaxial TiC/SiC multilayers deposited at ~550 °C were shown to contain cubic SiC layers up to a thickness of ~2 nm. Thicker SiC layers gives a-SiC due to the corresponding increase in interfacial strain energy leading to loss of coherent-layer growth. Nanoindentation of epitaxial Ti3SiC2/TiC0.67 nanolaminates showed inhibition of kink-band formation in Ti3SiC2, as the lamination with the less ductile TiC effectively hindered this mechanism.

Abstract [sv]

Materialteknik har alltid varit en central del av människans historia, och en förutsättning för utvecklingen av civilisationen. Dess betydelse märks inte minst på hur vi uppkallat historiska perioder efter vilka material som använts: stenåldern, bronsåldern och järnåldern (kiselåldern?). Modern materialvetenskap däremot handlar inte bara om att tillverka och utveckla material, utan även om att förstå sambandet mellan tillverknings¬processen, materialets struktur och dess egenskaper – samt hur denna förståelse kan användas för att designa material. I min avhandling sammanstrålar tre begrepp inom materialvetenskap, (multi-)funktionalitet, nanoteknik (nanostruktur) och tunna filmer.

Inom materialvetenskap och materialteknik skiljer man på begreppen strukturmaterial, som väljs ut för sin förmåga att bära en last (t.ex. byggmaterial) och funktionella material, där det intressanta är materialets funktion, t.ex. elektriska, magnetiska, optiska eller vissa mekaniska egenskaper. Multifunktionella material är material som är utvalda eller designade för att ha flera funktioner – exempelvis god elektrisk ledningsförmåga, nötningsmot-stånd och korrosionsmotstånd.

Nanoteknik handlar om material (strukturer, maskiner, etc…) där åtminstone någon dimension är på nanometerskalan (nanometer = miljarddels meter). Men det räcker inte med att enbart vara liten – nanoteknik betyder att man får nya funktioner tack vare storleken. I samhällsdebatten beskrivs nanoteknik ofta utifrån visioner om möjliga framtida kvantdatorer, molekylfabriker, medicinska ”cell-robotar”, och så vidare; det finns också negativa visioner som den om självkopierande nanorobotar som tar över världen och ut-rotar allt liv. Men om man ignorerar dessa långsiktiga och/eller långsökta visioner, så är det viktigt att inse att nanotekniken finns i våra vardagsliv redan idag, och det är framför allt som materialteknik som nanotekniken har lämnat snackstadiet och blivit verkstad. Många kommersiella produkter idag innehåller nanostrukturerade material, det vill säga material där nya funktioner uppnås genom att designa materialets struktur på nanonivå.

Anledningen att man ofta vill belägga en yta med ett lager av något annat är att ytbeläggningen förändrar – förhoppningsvis till det bättre! – egenskaperna hos det belagda objektet. Det är därför man målar huset eller lackerar köksbordet. Med tunna filmer menar man ytbeläggningar tunnare än någon eller några mikrometer (miljondels meter). Antireflexbehandlingen på glasögon och teflonet i stekpannan är några exempel från vardagen.

Processen jag använt kallas sputtring (egentligen heter det katodförstoftning på svenska, men ingen använder det ordet!), och äger rum i en vakuumkammare där trycket kan vara så lågt som en biljondel av atmosfärtrycket. Där placerar man det material man vill göra en tunnfilm av. Sedan släpper man in en gas, oftast en ädelgas som argon, som får bilda ett plasma, det vill säga en gas som mest består av laddade partiklar (joner). Argonjonerna accelereras med hög energi och får bombardera materialet; då slås atomer av ämnet ut och sprids i vakuumkammaren. De kan sedan kondensera på den yta man vill belägga och bilda en tunnfilm. En stor fördel med denna ”biljard på atomnivå” är att man har väldigt stora möjligheter att styra hur filmen bildas och växer, med andra ord går det att designa filmens struktur och i förlängningen dess egenskaper.

Det material jag studerat är titankiselkarbid, alltså ett ternärt material – det består av tre grundämnen (titan, kisel och kol). Varför ett så krångligt val – hade det inte varit mycket enklare att bara använda ett eller två grundämnen? Visst hade det varit enklare – men också tråkigare! Det blir visserligen mer komplicerat av att lägga till fler grundämnen, men flexibiliteten och designmöjligheterna ökar i motsvarande grad. I titankiselkarbid¬systemet kan jag tillverka en rad olika typer nanostrukturerade material, där de viktigaste kanske är Ti3SiC2, vars fascinerande struktur påminner om ett laminatgolv på nanonivå, och nanokompositer, med små titankarbidkristaller inbakade i amorft material. Båda dessa har unika egenskaper tack vare sin nanostruktur – de är hyfsade elektriska ledare, lagom hårda utan att vara för hårda, inte spröda, korrosionsbeständiga, och så vidare.

Kort sagt, de är Multifunktionella nanostrukturerade tunna filmer av titankiselkarbid!

Place, publisher, year, edition, pages
Institutionen för fysik, kemi och biologi , 2007.
Series
Linköping Studies in Science and Technology. Dissertations, ISSN 0345-7524 ; 1087
National Category
Other Engineering and Technologies not elsewhere specified
Identifiers
URN: urn:nbn:se:liu:diva-8860ISBN: 978-91-85715-31-2 (print)OAI: oai:DiVA.org:liu-8860DiVA: diva2:23570
Public defence
2007-04-20, Planck, F, 10:15 (English)
Opponent
Supervisors
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2016-08-31
List of papers
1. Homoepitaxial growth of Ti-Si-C MAX-phase thin films on bulk Ti3SiC2 substrates
Open this publication in new window or tab >>Homoepitaxial growth of Ti-Si-C MAX-phase thin films on bulk Ti3SiC2 substrates
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2007 (English)In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 304, no 1, 264-269 p.Article in journal (Refereed) Published
Abstract [en]

Ti3SiC2 films were grown on polycrystalline Ti3SiC2 bulk substrates using DC magnetron sputtering. The crystallographic orientation of the film grains is shown to be determined by the respective substrate-grain orientation through homoepitaxial MAX-phase growth. For a film composition close to Ti:Si:C=3:1:2, the films predominantly consist of MAX phases, both Ti3SiC2 and the metastable Ti4SiC3. Lower Si content resulted in growth of TiC with Ti3SiC2 as a minority phase. Thus, MAX-phase heterostructures with preferred crystallographic relationships can also be realized.

Keyword
Scanning electron microscopy, Transmission electron microscopy, X-ray diffraction, Physical vapor deposition processes, Carbides, Nanomaterials
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14471 (URN)10.1016/j.jcrysgro.2007.02.014 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
2. Magnetron sputtering of Ti3SiC2 thin films from a Ti3SiC2 compound target
Open this publication in new window or tab >>Magnetron sputtering of Ti3SiC2 thin films from a Ti3SiC2 compound target
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2007 (English)In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 25, no 5, 1381-1388 p.Article in journal (Refereed) Published
Abstract [en]

Ti3 Si C2 thin films were synthesized by magnetron sputtering from Ti3 Si C2 and Ti targets. Sputtering from a Ti3 Si C2 target alone resulted in films with a C content of ∼50 at. % or more, due to gas-phase scattering processes and differences in angular and energy distributions between species ejected from the target. Addition of Ti to the deposition flux from a Ti3 Si C2 target is shown to bind the excess C in Ti Cx intergrown with Ti3 Si C2 and Ti4 Si C3. Additionally, a substoichiometric Ti Cx buffer layer is shown to serve as a C sink and enable the growth of Ti3 Si C2.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14472 (URN)10.1116/1.2757178 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
3. Structural, electrical, and mechanical properties of nc-TiC/a-SiC nanocomposite thin films
Open this publication in new window or tab >>Structural, electrical, and mechanical properties of nc-TiC/a-SiC nanocomposite thin films
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2005 (English)In: Journal of Vacuum Science & Technology B, ISSN 1071-1023, E-ISSN 1520-8567, Vol. 23, no 6, 2486-2495 p.Article in journal (Refereed) Published
Abstract [en]

We have synthesized Ti–Si–C nanocomposite thin films by dc magnetron sputtering from a Ti3SiC2 compound target in an Ar discharge on Si(100), Al2O3(0001), and Al substrates at temperatures from room temperature to 300  °C. Electron microscopy, x-ray diffraction, and x-ray photoelectron spectroscopy showed that the films consisted of nanocrystalline (nc-) TiC and amorphous (a-) SiC, with the possible presence of a small amount of noncarbidic C. The growth mode was columnar, yielding a nodular film-surface morphology. Mechanically, the films exhibited a remarkable ductile behavior. Their nanoindentation hardness and E-modulus values were 20 and 290  GPa, respectively. The electrical resistivity was 330  µ  cm for optimal Ar pressure (4  mTorr) and substrate temperature (300  °C). The resulting nc-TiC/a-SiC films performed well as electrical contact material. These films' electrical-contact resistance against Ag was remarkably low, 6  µ at a contact force of 800  N compared to 3.2  µ for Ag against Ag. The chemical stability of the nc-TiC/a-SiC films was excellent, as shown by a Battelle flowing mixed corrosive-gas test, with no N, Cl, or S contaminants entering the bulk of the films.

Keyword
titanium compounds, silicon compounds, wide band gap semiconductors, nanocomposites, amorphous semiconductors, thin films, sputter deposition, electron microscopy, X-ray diffraction, X-ray photoelectron spectra, surface morphology, ductility, indentation, hardness, electrical resistivity, electrical contacts, contact resistance
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-14473 (URN)10.1116/1.2131081 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
4. Microstructure and electrical properties of Ti-Si-C-Ag nanocomposite thin films
Open this publication in new window or tab >>Microstructure and electrical properties of Ti-Si-C-Ag nanocomposite thin films
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2007 (English)In: Surface and Coatings Technology, ISSN 0257-8972, Vol. 201, no 14, 6465-6469 p.Article in journal (Refereed) Published
Abstract [en]

Ti–Si–C–Ag nanocomposite coatings consisting of nanocrystalline TiC in an amorphous Si matrix with segregated Ag were deposited by dual magnetron sputtering from Ti3SiC2 and Ag targets. As evidenced by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, for Ag contents below 10 at.%, the Ag forms 10 nm large crystallites that are homogeneously distributed in the films. For higher Ag contents, coalescence during growth results in the formation of >  100 nm Ag islands on the film surface. The electrical resistivity of the coatings was measured in a four-point-probe setup, and ranged from 340 μΩcm (for Ti–Si–C coatings without Ag) to 40 μΩcm (for high Ag content).

Keyword
Sputtering, Titanium carbide, Silver; Resistivity, X-ray diffraction, Electron microscopy
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-14474 (URN)10.1016/j.surfcoat.2006.12.016 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2016-08-31
5. High-power impulse magnetron sputtering of Ti-Si-C thin films from a Ti3SiC2 compound target
Open this publication in new window or tab >>High-power impulse magnetron sputtering of Ti-Si-C thin films from a Ti3SiC2 compound target
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2006 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 515, no 4, 1731-1736 p.Article in journal (Refereed) Published
Abstract [en]

We have deposited Ti-Si-C thin films using high-power impulse magnetron sputtering (HIPIMS) from a Ti3SiC2 compound target. The as-deposited films were composite materials with TiC as the main crystalline constituent. X-ray diffraction and photoelectron spectroscopy indicated that they also contained amorphous SiC, and for films deposited on inclined substrates, crystalline Ti5Si3Cx. The film morphology was dense and flat, while films deposited with dc magnetron sputtering under comparable conditions were rough and porous. Due to the high degree of ionization of the sputtered species obtained in HIPIMS, it is possible to control the film composition, in particular the C content, by tuning the substrate inclination angle, the Ar process pressure, and the bias voltage.

Place, publisher, year, edition, pages
Institutionen för fysik, kemi och biologi, 2006
Keyword
HIPIMS, Titanium silicon carbide
National Category
Physical Sciences
Identifiers
urn:nbn:se:liu:diva-10437 (URN)10.1016/j.tsf.2006.06.015 (DOI)000242931900079 ()
Note

Original publication: J. Alami, P. Eklund, J. Emmerlich, O. Wilhelmsson, U. Jansson, H. Högberg, L. Hultman, & U. Helmersson, High-power impulse magnetron sputtering of Ti-Si-C thin films from a Ti3SiC2 compound target, 2006, Thin Solid Films, (515), 4, 1731-1736. http://dx.doi.org/10.1016/j.tsf.2006.06.015. Copyright: Elsevier B.V., http://www.elsevier.com/.

Available from: 2007-12-14 Created: 2007-12-14 Last updated: 2017-12-14Bibliographically approved
6. Electrical resistivity of Tin+1ACn (A = Si, Ge, Sn, n = 1–3) thin films
Open this publication in new window or tab >>Electrical resistivity of Tin+1ACn (A = Si, Ge, Sn, n = 1–3) thin films
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2007 (English)In: Journal of Materials Research, ISSN 0884-2914, E-ISSN 2044-5326, Vol. 22, no 8, 2279-2287 p.Article in journal (Refereed) Published
Abstract [en]

We have investigated the electrical resistivity of (0001)-oriented Tin+1ACn (A = Si, Ge, Sn, n = 1–3) thin films deposited by magnetron sputtering onto Al2O3(0001) substrates at temperatures ranging from 500 to 950 °C. Four-point-probe measurements show that all films are good conductors with resistivity values of ∼21–51 μΩ cm for Ti–Si–C films, ∼15–50 μΩ cm for Ti–Ge–C films, and ∼46 μΩ cm for Ti2SnC. We find a general trend of decreasing resistivity with decreasing n for the Ti–Si–C and Ti–Ge–C systems due to the increased metallicity obtained with increasing density of A-element layers. We also show that crystalline quality and competitive growth of impurity phases affect the measured resistivity values. The effect of a given impurity phase largely depends on its location in the sample. Specifically, a TiCx layer in the center of the film constricts the current flow and results in an increased measured resistivity value. However, TiCx transition or seed layers at the substrate–film interface as well as surface segregation of Ge and Ti5Ge3Cx (for Ti–Ge–C) have only little effect on the measured resistivity values. For the Ti–Sn–C system, the resistivity is mainly influenced by the segregation of metallic Sn, yielding a wide spread in the measured values ranging from 20–46 μΩ cm, in the order of increased film purity.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14476 (URN)10.1557/jmr.2007.0284 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
7. Photoemission studies of Ti3SiC2 and nanocrystalline-TiC/amorphous-SiC nanocomposite thin films
Open this publication in new window or tab >>Photoemission studies of Ti3SiC2 and nanocrystalline-TiC/amorphous-SiC nanocomposite thin films
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2006 (English)In: Physical Review B. Condensed Matter and Materials Physics, ISSN 1098-0121, E-ISSN 1550-235X, Vol. 74, no 4, 045417- p.Article in journal (Refereed) Published
Abstract [en]

Photoemissionstudies using synchrotron radiation have been performed on epitaxial Ti3SiC2(0001)and compound nanocrystalline (nc-)TiC/amorphous (a-)SiC thin films deposited by magnetronsputtering. As-introduced samples were found to be covered by surfaceoxides, SiOx and TiOx. These oxides could be removed byin-situ annealing to ~1000  °C. For as-annealed Ti3SiC2(0001), surface Si wasobserved and interpreted as originating from decomposition of Ti3SiC2 throughSi out-diffusion. For nc-TiC/a-SiC annealed in situ to ~1000  °C, thesurface instead exhibited a dominant contribution from graphitic carbon, alsowith the presence of Si, due to C and Siout-diffusion from the a-SiC compound or from grain boundaries.

Keyword
titanium compounds, silicon compounds, wide band gap semiconductors, nanocomposites, amorphous state, epitaxial layers, sputtered coatings, photoelectron spectra, surface composition, annealing, decomposition, surface diffusion, grain boundaries
National Category
Engineering and Technology
Identifiers
urn:nbn:se:liu:diva-14477 (URN)10.1103/PhysRevB.74.045417 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
8. Thermal stability of Ti3SiC2 thin films
Open this publication in new window or tab >>Thermal stability of Ti3SiC2 thin films
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2007 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 55, no 4, 1479-1488 p.Article in journal (Refereed) Published
Abstract [en]

The thermal stability of Ti3SiC2(0 0 0 1) thin films is studied by in situ X-ray diffraction analysis during vacuum furnace annealing in combination with X-ray photoelectron spectroscopy, transmission electron microscopy and scanning transmission electron microscopy with energy dispersive X-ray analysis. The films are found to be stable during annealing at temperatures up to ∼1000 °C for 25 h. Annealing at 1100–1200 °C results in the rapid decomposition of Ti3SiC2 by Si out-diffusion along the basal planes via domain boundaries to the free surface with subsequent evaporation. As a consequence, the material shrinks by the relaxation of the Ti3C2 slabs and, it is proposed, by an in-diffusion of O into the empty Si-mirror planes. The phase transformation process is followed by the detwinning of the as-relaxed Ti3C2 slabs into (1 1 1)-oriented TiC0.67 layers, which begin recrystallizing at 1300 °C. Ab initio calculations are provided supporting the presented decomposition mechanisms.

Keyword
Ti3SiC2 thin films, Phase transformations, X-ray diffraction, Transmission electron microscopy, Ab initio electron theory
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14478 (URN)10.1016/j.actamat.2006.10.010 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13
9. Epitaxial TiC/SiC multilayers
Open this publication in new window or tab >>Epitaxial TiC/SiC multilayers
2007 (English)In: Physica status solidi (RRL): rapid research letters, ISSN 1862-6254, Vol. 1, no 3, 113-115 p.Article in journal (Refereed) Published
Abstract [en]

Epitaxial TiC/SiC multilayers were grown by magnetron sputtering at a substrate temperature of 550 °C, where SiC is normally amorphous. The epitaxial TiC template induced growth of cubic SiC up to a thickness of ~2 nm. Thicker SiC layers result in a direct transition to growth of the metastable amorphous SiC followed by renucleation of nanocrystalline TiC layers

Keyword
61.10.Nz, 68.37.Lp, 68.55.-a, 81.05.Je, 81.07.Bk, 81.15.Kk
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14479 (URN)10.1002/pssr.200701027 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2016-08-31
10. Intrusion-type deformation in epitaxial Ti3SiC2/TiCx nanolaminates
Open this publication in new window or tab >>Intrusion-type deformation in epitaxial Ti3SiC2/TiCx nanolaminates
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2007 (English)In: Applied Physics Letters, ISSN 0003-6951, E-ISSN 1077-3118, Vol. 91, no 12, 123124- p.Article in journal (Refereed) Published
Abstract [en]

We investigate the deformation of epitaxial Ti3 Si C2 (0001) Ti Cx (111) (x∼0.67) nanolaminates deposited by magnetron sputtering. Nanoindentation and transmission electron microscopy show that the Ti3 Si C2 layers deform via basal plane slip and intrusion into the TiC layers, suppressing kink-band and pile-up deformation behaviors analogous with monolithic Ti3 Si C2. This remarkable response to indentation is due to persistent slip in the TiC layers and prevention of gross slip throughout the nanolaminate by the interleaving Ti3 Si C2 layers. Hardness and Young's modulus were measured as ∼15 and ∼240 GPa, respectively.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-14480 (URN)10.1063/1.2789710 (DOI)
Available from: 2007-05-14 Created: 2007-05-14 Last updated: 2017-12-13

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