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  • 1.
    Abrikosov, Igor
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Knutsson, Axel
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Alling, Björn
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Tasnádi, Ferenc
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Lind, Hans
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Phase Stability and Elasticity of TiAlN2011Ingår i: Materials, ISSN 1996-1944, E-ISSN 1996-1944, Vol. 4, nr 9, s. 1599-1618Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    We review results of recent combined theoretical and experimental studies of Ti1−xAlxN, an archetypical alloy system material for hard-coating applications. Theoretical simulations of lattice parameters, mixing enthalpies, and elastic properties are presented. Calculated phase diagrams at ambient pressure, as well as at pressure of 10 GPa, show a wide miscibility gap and broad region of compositions and temperatures where the spinodal decomposition takes place. The strong dependence of the elastic properties and sound wave anisotropy on the Al-content offers detailed understanding of the spinodal decomposition and age hardening in Ti1−xAlxN alloy films and multilayers. TiAlN/TiN multilayers can further improve the hardness and thermal stability compared to TiAlN since they offer means to influence the kinetics of the favorable spinodal decomposition and suppress the detrimental transformation to w-AlN. Here, we show that a 100 degree improvement in terms of w-AlN suppression can be achieved, which is of importance when the coating is used as a protective coating on metal cutting inserts.

  • 2.
    Alling, Björn
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Abrikosov, Igor
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Teoretisk Fysik. Linköpings universitet, Tekniska högskolan.
    Pressure enhancement of the isostructural cubic decomposition in Ti1−xAlxN2009Ingår i: Applied Physics Letters, ISSN 0003-6951, E-ISSN 1077-3118, Vol. 95, nr 181906Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The influence of pressure on the phase stabilities of Ti1−xAlxN solid solutions has been studied using first principles calculations. We find that the application of hydrostatic pressure enhances the tendency for isostructural decomposition, including spinodal decomposition. The effect originates in the gradual pressure stabilization of cubic AlN with respect to the wurtzite structure and an increased isostructural cubic mixing enthalpy with increased pressure. The influence is sufficiently strong in the composition-temperature interval corresponding to a shoulder of the spinodal line that it could impact the stability of the material at pressures achievable in the tool-work piece contact during cutting operations

  • 3.
    Almer, J.
    et al.
    Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois.
    Lienert, U
    Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois.
    Peng, Ru
    Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial. Linköpings universitet, Tekniska högskolan.
    Schlauer, Christian
    Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Engineering Materials Luleå University of Technology.
    Strain and texture analysis of coatings using high-energy x-rays2003Ingår i: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 94, nr 1, s. 697-702Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    We investigate the internal strain and crystallographic orientation (texture) in physical-vapor deposited metal nitride coatings of TiN and CrN. A high-energy diffraction technique is presented that uses synchrotron x rays and an area detector, and which allows the strain and intensity distributions of multiple crystallographic planes to be measured by a single x-ray exposure. Unique texture states and nonlinear sin2 ψ strain distributions are observed for all coatings investigated. Quantitative analysis indicates that existing micromechanical models can reasonably predict strain and corresponding stress for mixed-hkl reflections but are inadequate for fully describing measured data. Alternative mechanisms involving deposition-induced defects are proposed.

  • 4. Almer, J
    et al.
    Odén, Magnus
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material.
    Hakansson, G
    Microstructure and thermal stability of arc-evaporated Cr-C-N coatings2004Ingår i: PHILOSOPHICAL MAGAZINE, ISSN 1478-6443, Vol. 84, nr 7, s. 611-630Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The role of C incorporation in the microstructure and thermal stability of arc-evaporated Cr-C-N coatings is explored via reactive growth in a mixed C2H4-N-2 environment. C is found to react more readily than N at both the Cr cathode and the coating surfaces, so that a C2H4-to-N-2 flow ratio of only 1% yields a C-to-N ratio of approximately 10% within the coatings. The as-deposited microstructures consist primarily of the delta-Cr(C, N) phase and possess high compressive residual stresses, which decrease with increasing C content. Post-deposition annealing up to 700degreesC results in depletion of lattice defects, and concomitant reductions in stress and coating hardness, together with phase transformations which suggest metastable phase formation during growth. Apparent activation energies for this lattice defect are found to be in the range expected for bulk diffusion of N and C (2.4-2.8 eV). The results suggest that inclusion of small amounts of C in this system offers the ability to reduce internal stresses while maintaining defect-related hardness increases, permitting growth of thicker and thus more wear-resistant coatings.

  • 5.
    Almer, J
    et al.
    Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial.
    Håkansson, G
    Bodycote Värmebehandling AB Linköping.
    Microstructure, stress and mechanical properties of arc-evaporated Cr-C-N coatings2001Ingår i: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 385, nr 1-2, s. 190-197Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The relationships between coating microstructure and properties in the Cr-C-N system have been investigated as a function of composition and post-deposition annealing. Coatings of varying compositions were grown using arc-evaporation, by varying the reactive gas flow ratio fR = f(C2H4)/f(N2) from 0 to 0.2, and were found to consist primarily of the cubic d-Cr(C,N) phase. Changes in both the unstressed lattice parameter, ao, and X-ray diffraction background intensity indicate that both the carbon concentration within the d-phase and amorphous/crystalline content increases with fR. Increasing fR also decreases the magnitude of the compressive biaxial residual stress, from approximately 6 to 1 GPa, while increasing both the inhomogeneous stress and thermal stability. The elastic modulus and hardness of as-deposited coatings were determined from nanoindentation to be 320 and 23 GPa, respectively, for moderate carbon concentrations (fR=0.05). Concurrent variations in microstructure and hardness with post-deposition annealing indicate that the as-deposited hardness is significantly enhanced by the microstructure, primarily by lattice defects and related stresses (microstresses) rather than average stresses (macrostresses).

  • 6.
    Almer, Jonathan
    et al.
    IKP, Konstruktionsmaterial Linköpings universitet.
    Odén, Magnus
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial.
    Hultman, Lars
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik.
    Håkansson, Greger
    Tixon Brukens Sverige AB Linköping.
    Microstructural evolution during tempering of arc-evaporated Cr-N coatings2000Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 18, nr 1, s. 121-130Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Cr-N coatings were arc-deposited at 50 and 300 V. The changes in the coating microstructure and phase content during tempering were monitored. As a result, the phase stability and activation energies for defect diffusion were determined as a function of ion energy.

  • 7. Almér, J.
    et al.
    Odén, Magnus
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för konstruktions- och produktionsteknik, Konstruktionsmaterial.
    Håkansson, G.
    Microstructure, Stress and Mechanical Properties in Arc-evaporated Cr-C-N Coatings2000Ingår i: Thin solid films : an international journal on the science and technology of thin and thick films, ISSN 0563-4652Artikel i tidskrift (Refereegranskat)
  • 8.
    Amini, Shahram
    et al.
    Drexel University.
    Cordoba Gallego, Jose M
    Los Alamos National Laboratory.
    McGhie, Andrew R
    University of Pennsylvania.
    Ni, Chaoying
    University of Delaware.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Oden, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    On the Stability of Mg Nanograins to Coarsening after Repeated Melting2009Ingår i: NANO LETTERS, ISSN 1530-6984, Vol. 9, nr 8, s. 3082-3086Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Herein we report on the extraordinary thermal stability of similar to 35 nm Mg-nanograins that constitute the matrix of a Ti2AlC-Mg composite that has previously been shown to have excellent mechanical properties. The microstructure is so stable that heating the composite three times to 700 degrees C, which is 50 degrees C over the melting point of Mg, not only resulted in the repeated melting of the Mg, but surprisingly and within the resolution of our differential scanning calorimeter, did not lead to any coarsening. The reduction in the Mg melting point due to the nanograins was similar to 50 degrees C. X-ray diffraction and neutron spectroscopy results suggest that thin, amorphous, and/or poorly crystallized rutile, anatase, and/or magnesia layers separate the Mg nanograins and prevent them from coarsening. Clearly that layer is thin enough, and thus mechanically robust enough, to survive the melting and solidification stresses encountered during cycling. Annealing in hydrogen at 250 degrees C for 20 h, also did not seem to alter the grain size significantly.

  • 9.
    Antti, M.-L.
    et al.
    Luleå University of Technology.
    Cheng, Y.-B.
    Monash University.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Synthesis and phase development in the Ct-Al-N system2009Ingår i: Ceramic Engineering and Science Proceedings, vol 29, no 2, 2009, Vol. 29, nr 2, s. 3-12Konferensbidrag (Refereegranskat)
    Abstract [en]

    The ternary nitride system Cr-Al-N has been investigated by sintering different powder compositions. The powder compositions belong to four groups, AIN- + Cr-powder (5 compositions between 20-90 molar% AlN), Al- + Cr 2N-powder (5 compositions between 15-80 molar% Cr2N), AlN-+ Cr2N-powder (50- and 90 molar% Cr2N) and Al- + Cr-powder. The powders were dry mixed and pressed into pellets by uniaxial pressing followed by cold isostatic pressing (ClP). Sintering took place in a graphite lined reaction bonding furnace under nitrogen atmosphere at three different temperatures, 1350C, 1500C and 1800C and in an alumina tube furnace in order to avoid access to carbon. Holding times were varied, from 2 hours up to 72 hours. The phase development was evaluated by thermal analysis and XRD. CrAlN was formed at 1350C but decomposed at higher temperatures. Both pure Al and Cr-powder were prone to react with carbon in the graphite furnace. Thermal analysis showed a sublimation of Cr2N at temperatures around 1050C and nitridation of pure Al-powder between 680-750C and of pure Cr-powder between 610-1080C. Samples with pure Al-powder showed a very large expansion due to melting of aluminium in combination with nitridation. AIN was found to be more stable than Cr 2N at higher temperatures and longer holding times. The mixtures of Al-+Cr-powder produced an intermediate Al-Cr-phase.

  • 10.
    Asp Grönhagen, Klara
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Agren, J.
    Royal Institute Technology, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Phase-field modelling of spinodal decomposition in TiAlN including the effect of metal vacancies2015Ingår i: Scripta Materialia, ISSN 1359-6462, E-ISSN 1872-8456, Vol. 95, s. 42-45Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Using a CALPHAD approach together with a Cahn-Hilliard model, we describe the microstructure evolution in cubic Ti1-xAlxN including vacancies on the metal sublattice. Our results show that vacancy content has a pronounced effect on the decomposition kinetics. Furthermore, vacancies show a strong tendency to segregate to the coherent AlN-TiN interface regions. We illustrate how vacancies anneal to grain boundaries, and finally, we compare our prediction to experimental differential scanning calorimetry data and attribute the second peak in the thermogram to vacancy depletion.

  • 11.
    Atakan, Aylin
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Erdtman, Edvin
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Mäkie, Peter
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Ojamäe, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Time evolution of the CO2 hydrogenation to fuels over Cu-Zr-SBA-15 catalysts2018Ingår i: Journal of Catalysis, ISSN 0021-9517, E-ISSN 1090-2694, Vol. 362, s. 55-64Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Time evolution of catalytic CO2 hydrogenation to methanol and dimethyl ether (DME) has been investigated in a high-temperature high-pressure reaction chamber where products accumulate over time. The employed catalysts are based on a nano-assembly composed of Cu nanoparticles infiltrated into a Zr doped SiOx mesoporous framework (SBA-15): Cu-Zr-SBA-15. The CO2 conversion was recorded as a function of time by gas chromatography-mass spectrometry (GC-MS) and the molecular activity on the catalyst’s surface was examined by diffuse reflectance in-situ Fourier transform infrared spectroscopy (DRIFTS). The experimental results showed that after 14 days a CO2 conversion of 25% to methanol and DME was reached when a DME selective catalyst was used which was also illustrated by thermodynamic equilibrium calculations. With higher Zr content in the catalyst, greater selectivity for methanol and a total 9.5% conversion to methanol and DME was observed, yielding also CO as an additional product. The time evolution profiles indicated that DME is formed directly from methoxy groups in this reaction system. Both DME and methanol selective systems show the thermodynamically highest possible conversion.

  • 12.
    Atakan, Aylin
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Keraudy, Julien
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Mäkie, Peter
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Hulteberg, Christian
    Lund Univ, Sweden.
    Björk, Emma
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Impact of the morphological and chemical properties of copper-zirconium-SBA-15 catalysts on the conversion and selectivity in carbon dioxide hydrogenation2019Ingår i: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 546, s. 163-173Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    A hybrid catalyst consisting of Zr-doped mesoporous silica (Zr-SBA-15) supports with intergrown Cu nanoparticles was used to study the effects of a catalysts chemical states on CO2 hydrogenation. The chemical state of the catalyst was altered by using tetraethyl orthosilicate (TEOS) or sodium metasilicate (SMS) as the silica precursor in the synthesis of the Zr-SBA-15 framework, and infiltration (Inf) or evaporation induced wetness impregnation (EIWI) as the Cu loading method. As a result, the silica precursor mainly affects the activity of the catalyst whereas the Cu loading method alters the selectivity of the products. TEOS materials exhibit a higher catalytic activity compared to SMS materials due to different Zr dispersion and bonding to the silica matrix. EIWI catalysts display selectivity for methanol formation, while the Inf ones enable methanol conversion to DME. This is correlated to a higher Zr content and lower Cu oxidation states of EIWI prepared catalysts. (C) 2019 Elsevier Inc. All rights reserved.

  • 13.
    Atakan, Aylin
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Mäkie, Peter
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Keraudy, Julien
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Johansson, Emma
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Synthesis of a Cu-infiltrated Zr-doped SBA-15 catalyst for CO2 hydrogenation into methanol and dimethyl ethert2017Ingår i: Physical Chemistry, Chemical Physics - PCCP, ISSN 1463-9076, E-ISSN 1463-9084, Vol. 19, nr 29, s. 19139-19149Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    A catalytically active nanoassembly comprising Cu-nanoparticles grown on integrated and active supports (large pore Zr-doped mesoporous SBA-15 silica) has been synthesized and used to promote CO2 hydrogenation. The doped mesoporous material was synthesized using a sal-gel method, in which the pore size was tuned between 11 and 15 nm while maintaining a specific surface area of about 700 m(2) g (1). The subsequent Cu nanoparticle growth was achieved by an infiltration process involving attachment of different functional groups on the external and internal surfaces of the mesoporous structure such that 7-10 nm sized Cu nanoparticles grew preferentially inside the pores. Chemisorption showed improved absorption of both CO2 and H-2 for the assembly compared to pure SBA-15 and 15% of the total CO2 was converted to methanol and dimethyl ether at 250 degrees C and 33 bar.

  • 14.
    Ballem, Mohamed A.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Córdoba, José M.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Influence of synthesis temperature on morphology of SBA-16 mesoporous materials with a three-dimensional pore system2010Ingår i: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 129, s. 106-111Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Spherical particles of mesoporous silica SBA-16 with cubic Im3m structure were synthesized at low pH using Pluronic F127 as template and TEOS as silica source. The diameter of the spherical particles can be controlled in the range of 0.5–8 μm by varying synthesis temperature from 1 °C up to 40 °C. A sharp transition from large particle sizes at approximately 20 °C to smaller ones is observed when the temperature is increased. It is suggested that this morphology transition is due to a change in hydrolysis and condensation rate of the silica source and as a result the assembly of F127 micelles will differ. The SBA-16 samples were characterized using powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption techniques.

  • 15.
    Ballem, Mohamed A.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Córdoba, José
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Mesoporous silica templated zirconia nanoparticles2011Ingår i: Journal of nanoparticle research, ISSN 1388-0764, E-ISSN 1572-896X, Vol. 13, nr 7, s. 2743-2748Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Nanoparticles of zirconium oxide (ZrO2)were synthesized by infiltration of a zirconia precursor(ZrOCl28H2O) into a SBA-15 mesoporous silicamold using a wet-impregnation technique. X-raydiffractometry and high-resolution transmission electronmicroscopy show formation of stable ZrO2nanoparticles inside the silica pores after a thermaltreatment at 550 C. Subsequent leaching out of thesilica template by NaOH resulted in well-dispersedZrO2 nanoparticles with an average diameter of*4 nm. The formed single crystal nanoparticles arefaceted with 110 surfaces termination suggesting it tobe the preferred growth orientation. A growth modelof these nanoparticles is also suggested.

  • 16.
    Ballem, Mohamed A.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Zhang, Xuanjun
    Linköpings universitet, Tekniska högskolan. Linköpings universitet, Institutionen för fysik, kemi och biologi, Tillämpad Fysik.
    Johansson, Emma M.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Córdoba, José M.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Low Temperature Nanocasting of Ultrafine Hematite Nanoparticles using Mesoporous Silica Molds2012Ingår i: Powder Technology, ISSN 0032-5910, E-ISSN 1873-328X, Vol. 217, s. 269-273Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Iron oxide (α-Fe2O3) nanoparticles with very small size, high crystallinity, and narrow size distribution were synthesized by infiltration of Fe(NO3)3.9H2O as an oxide precursor into mesoporous silica (SBA-15 and SBA-16) molds using a wetimpregnation technique. High resolution transmission electron microscopy shows that during the hydrothermal treatment of the precursor at 140 °C for 2 days, stable α-Fe2O3 nanoparticles inside the silica pores are formed. Subsequent leaching out of the silica template by NaOH resulted in well dispersed nanoparticles with an average diameter of ~ 4 nm.

  • 17.
    Ballem, Mohamed Ali
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Nordblad, Per
    Uppsala Unversity, Sweden.
    Käll, Per-Olov
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Growth of Gd2O3 nanoparticles inside mesoporous silica frameworks2013Ingår i: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 168, s. 221-224Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Gadolinium oxide (Gd2O3) nanoparticles with very small size, and narrow size distribution were synthesized by infiltration of Gd(NO3)3.6H2O as an oxide precursor into the pores of SBA-15 mesoporous silica using a wet-impregnation technique. High resolution transmission electron microscopy and X-ray diffraction show that during the hydrothermal treatment of the precursor at 550 °C, gadolinium oxide nanoparticles inside the silica pores are formed. Subsequent dissolution of the silica template by NaOH resulted in well dispersed nanoparticles with an average diameter of 3.6 ± 0.9 nm.

  • 18.
    Ballem, Mohamed
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Johansson, Emma
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Cordoba Gallego, Jose Manuel
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Synthesis of hollow silica spheres SBA-16 with large-pore diameter2011Ingår i: Materials letters (General ed.), ISSN 0167-577X, E-ISSN 1873-4979, Vol. 65, nr 7, s. 1066-1068Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Hollow silica SBA-16 spheres with cubic ordered mesoporous shells were synthesized by an emulsion-templating method, using Pluronic F127 as a structure-directing agent. tetraethyl orthosilicateas as a silica source and heptane as a cosolvent in the presence of NH4F. The size of these spheres is in the range of 10 to 30 mu m. The shell is about 700 nm thick and consists of large pores, similar to 9 nm in diameter, arranged in a cubic order. After calcination, the spheres maintain their mesoporosity and show a high surface area of 822 m(2)/g. The formation mechanism of the silica hollow spheres is discussed.

  • 19.
    Barrirero, J.
    et al.
    Saarland Univ, Germany.
    Engstler, M.
    Saarland Univ, Germany.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Muecklich, F.
    Saarland Univ, Germany.
    Phase Selective Sample Preparation of Al-Si alloys for Atom Probe Tomography2019Ingår i: Praktische metallographie, ISSN 0032-678X, E-ISSN 2195-8599, Vol. 56, nr 2, s. 76-90Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    We present how the conventional focused ion beam (FIB) lift-out method can be modified to obtain phase selective specimens for atom probe tomography (APT). The modified method combines selective deep etching with site-specific lift-out using a micromanipulator in a FIB/SEM workstation. This method is used for phase-selective sample preparation in alloys with complex microstructures such as the coral- and plate-like silicon structures in the eutectic phase of Al-Si castings. The method proves to be both, practical and robust, with a high success rate of high-quality phase-specific APT specimens.

  • 20.
    Barrirero, Jenifer
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan. Saarland University, Saarbrücken, Germany.
    Engstler, Michael
    Saarland University, Saarbrücken, Germany.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    de Jonge, Niels
    Saarland University, Saarbrücken, Germany.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Muecklich, Frank
    Saarland University, Saarbrücken, Germany.
    Comparison of segregations formed in unmodified and Sr-modified Al-Si alloys studied by atom probe tomography and transmission electron microscopy2014Ingår i: Journal of Alloys and Compounds, ISSN 0925-8388, E-ISSN 1873-4669, Vol. 611, s. 410-421Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The mechanical properties of Al-7 wt.% Si can be enhanced by structural modifications of its eutectic phase. Addition of low concentrations of certain elements, in this case 150 wt-ppm Sr, is enough to cause a transition from a coarse plate-like Si structure to a finer coralline one. To fully understand the operating mechanism of this modification, the composition of the eutectic Si phase in unmodified and Sr-modified alloys was analysed and compared by atom probe tomography and (scanning) transmission electron microscopy. The unmodified alloy showed nanometre sized Al-segregations decorating defects, while the Sr-modified sample presented three types of Al-Sr segregations: (1) rod-like segregations that promote smoothening of the Al-Si boundaries in the eutectic phase, (2) particle-like segregations comparable to the ones seen in the unmodified alloy, and (3) planar segregations favouring the formation of twin boundaries. Al and Sr solubilities in Si after solidification were determined to be 430 +/- 160 at-ppm and 40 +/- 10 at-ppm, respectively. Sr predominantly segregates to the Si phase confirming its importance in the modification of the eutectic growth.

  • 21.
    Barrirero, Jenifer
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi. Linköpings universitet, Tekniska fakulteten. University of Saarland, Germany.
    Li, Jiehua
    University of Leoben, Austria.
    Engstler, Michael
    University of Saarland, Germany.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Schumacher, Peter
    University of Leoben, Austria.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Muecklich, Frank
    University of Saarland, Germany.
    Cluster formation at the Si/liquid interface in Sr and Na modified Al-Si alloys2016Ingår i: Scripta Materialia, ISSN 1359-6462, E-ISSN 1872-8456, Vol. 117, s. 16-19Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Atom probe tomography was used to compare Na and Sr modified Al-Si hypoeutectic alloys. Both Na and Sr promote the formation of nanometre-sized clusters in the Si eutectic phase. Compositional analyses of the clusters show an Al:Sr ratio of 2.92 +/- 0.46 and an Al:Na ratio of 1.07 +/- 0.23. It is proposed that SrAl2Si2 and NaAlSi clusters are formed at the Si/liquid interface and take part in the modification process by altering the eutectic Si growth.

  • 22.
    Barrirero, Jenifer
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Saarland Univ, Germany.
    Pauly, C.
    Saarland Univ, Germany.
    Engstler, M.
    Saarland Univ, Germany.
    Ghanbaja, J.
    Univ Lorraine, France.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Li, J.
    Univ Leoben, Austria.
    Schumacher, P.
    Univ Leoben, Austria.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Muecklich, F.
    Saarland Univ, Germany.
    Eutectic modification by ternary compound cluster formation in Al-Si alloys2019Ingår i: Scientific Reports, ISSN 2045-2322, E-ISSN 2045-2322, Vol. 9, artikel-id 5506Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Al-alloys with Si as the main alloying element constitute the vast majority of Al castings used commercially today. The eutectic Si microstructure in these alloys can be modified from plate-like to coral-like by the addition of a small amount of a third element to improve ductility and toughness. In this investigation the effects of Eu and Yb are studied and their influence on the microstructure is compared to further understand this modification. The two elements impact the alloy differently, where Eu modifies Si into a coral-like structure while Yb does not. Atom probe tomography shows that Eu is present within the Si phase in the form of ternary compound Al2Si2Eu clusters, while Yb is absent in the Si phase. This indicates that the presence of ternary compound clusters within Si is a necessary condition for the formation of a coral-like structure. A crystallographic orientation relationship between Si and the Al2Si2Eu phase was found, where the following plane normals are parallel: 011(Si) //0001(Al2Si2Eu), 111(Si)//6 (7) over bar 10(Al2Si2Eu) and 011(Si)//6 (7) over bar 10(Al2Si2Eu). No crystallographic relationship was found between Si and Al2Si2Yb. The heterogeneous formation of coherent Al2Si2Eu clusters inside the Si-phase is suggested to trigger the modification of the microstructure.

  • 23.
    Björk, Emma M.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Grafting mesoporous silica particles to substrates: a method for synthesizing mesoporous films with cylindrical pores perpendicular to the substrate2013Manuskript (preprint) (Övrigt vetenskapligt)
    Abstract [en]

    A method for synthesizing mesoporous silica films with cylindrical pores perpendicular to the substrate has been developed. The films consist of SBA-15 platelets that are grafted on glass substrates. The grafting is studied in terms of parameters such as pH, substrate functionalization, salt additions, time for TEOS prehydrolysis, and calcination. The best coverage of particles on the substrate was achieved for a low pH in combination with OTS-treated glass substrate. Furthermore, the prehydrolysis time of the TEOS was found to be a key parameter in order to bind the particles to the substrate. These porous films have potential in applications such as catalysis, drug delivery, and as a template for nanoparticle or nanorod, growth.

  • 24.
    Björk, Emma M.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Single-pot synthesis of ordered mesoporous silica films with unique controllable morphology2014Ingår i: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 413, s. 1-7Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Mesoporous silica films consisting of a monolayer of separated SBA-15 particles with unusually wide and short pores grown on silicon wafers have been fabricated in a simple single-pot-synthesis, and the formation of the films has been studied. A recipe for synthesizing mesoporous silica rods with the addition of heptane and NH4F at low temperature was used and substrates were added to the synthesis solution during the reaction. The films are ∼90 nm thick, have a pore size of 10.7–13.9 nm depending on the hydrothermal treatment time and temperature, and a pore length of 200–400 nm. All pores are parallel to the substrate, open, and easy to access, making them suitable for applications such as catalyst hosts and gas separation. The growth of the films is closely correlated to the evolution of the mesoporous silica particles. Here, we have studied the time for adding substrates to the synthesis solution, the evolution of the films with time during formation, and the effect of hydrothermal treatment. It was found that the substrates should be added within 30–60 s after turning off the stirring and the films are formed within 10 min after addition to the synthesis solution. The study has yielded a new route for synthesizing mesoporous silica films with a unique morphology.

  • 25.
    Björk, Emma M.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Tuning the shape of mesoporous silica particles by alterations in parameter space: from rods to platelets2013Ingår i: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 29, nr 44, s. 13551-13561Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The knowledge of how to control the pore size and morphology of separated mesoporous silica particles is crucial for optimizing their performance in applications, such as molecular sieves and drug delivery systems. In this work, we have systematically studied the effects of various synthesis parameters to gain a deeper understanding of how particle morphologies can be altered. It was found that the morphology for isolated particles of SBA-15 type, with unusually short and wide pores, could be altered from rods to platelets by variations in the NH4F concentration. The pore length is nearly constant (similar to 300 nm) for the different morphologies, but the particle width is increasing from 200 nm to >3 mu m when decreasing the amount of NH4F, and the pore size can be tuned between 10 and 13 nm. Furthermore, other synthesis parameters such as heptane concentration, pH, silica precursor, and additions of ions have also been studied. The trend regarding particle width is independent of heptane concentration, at the same time as heptane increases the particle length up to a plateau value of similar to 500 nm. In all, parameters controlling particle width, length, and pore size have been separated in order to evaluate their function in the particle formation. Additionally, it was found that the formation time of the particles is strongly affected by the fluoride ion concentration, and a mechanism for particle formation for this system, where micelles transform from a foam, to multilamellar vesicles, and finally to cylindrical micelles, is suggested.

  • 26.
    Björk, Emma
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. University of Nacl Rio Cuarto, Argentina.
    Militello, Maria P.
    University of Nacl Rio Cuarto, Argentina.
    Tamborini, Luciano H.
    University of Nacl Rio Cuarto, Argentina.
    Coneo Rodriguez, Rusbel
    University of Nacl Rio Cuarto, Argentina.
    Planes, Gabriel A.
    University of Nacl Rio Cuarto, Argentina.
    Acevedo, Diego F.
    University of Nacl Rio Cuarto, Argentina; University of Nacl Rio Cuarto, Argentina.
    Sergio Moreno, M.
    Consejo Nacl Invest Cient and Tecn, Argentina.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Barbero, Cesar A.
    University of Nacl Rio Cuarto, Argentina.
    Mesoporous silica and carbon based catalysts for esterification and biodiesel fabrication-The effect of matrix surface composition and porosity2017Ingår i: Applied Catalysis A: General, ISSN 0926-860X, E-ISSN 1873-3875, Vol. 533, s. 49-58Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The effects of catalyst matrix porosity composition on the catalytic performance have been studied using sulfonated mesoporous SBA-15 silica. The matrix was sulfonated with three different methods grafting, in situ oxidation, and carbon infiltration. Additionally, unordered sulfonated mesoporous carbon, and the commercial catalysts Amberlite IR-120 and Nafion 117 were tested. The catalytic performance was evaluated in a Fischer esterification using acetic acid and ethanol, as well as in a transesterification of triglycerides (sunflower oil) and ethanol to produce biodiesel. The study shows that for long carbon chains, the effective wetting of the porous catalyst matrix by the reactants is most important for the catalytic efficiency, while for shorter carbon chain, the mass transport of the reagents trough the porous structure is more important. The catalysts were analysed using electron microscopy and physisorption. The study shows that the reactions are faster with carbon infiltrated materials than the silica materials due to a higher concentration of sulfonic groups linked to the carbon. The in situ functionalized SBA-15 is a more efficient catalyst compared to the post grafted one. All the synthesized catalysts outperform the commercial ones in both reactions in terms of conversion. (C) 2017 Elsevier B.V. All rights reserved.

  • 27.
    Björk, Emma
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Univ Ulm, Germany.
    Mäkie, Peter
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Rogström, Lina
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Atakan, Aylin
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Schell, Norbert
    Helmholtz Zentrum Geesthacht, Germany.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Formation of block-copolymer-templated mesoporous silica2018Ingår i: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 521, s. 183-189Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    In situ attenuated total reflectance Fourier transform infrared spectroscopy is used to monitor the chemical evolution of the mesoporous silica SBA-15 from hydrolysis of the silica precursor to final silica condensation after the particle formation. Two silica precursors, tetraethyl orthosilicate (TEOS) or sodium metasilicate (SMS) were used, and the effects of additive (heptane and NH4F) concentrations were studied. Five formation stages are identified when TEOS is used as the precursor. The fourth stage correlates with the appearance and evolution of diffraction peaks recorded using in situ small angle X-ray diffraction. Details of the formed silica matrix are observed, e.g. the ratio between six-fold cyclic silica rings and linear bonding increases with the NH4F concentration. The TEOS hydrolysis time is independent of the NH4F concentration for small amounts of heptane, but is affected by the size of the emulsion droplets when the heptane amount increases. Polymerization and condensation rates of both silica precursors are affected by the salt concentration. Materials synthesized using SMS form significantly faster compared to TEOS-materials due to the pre-hydrolysis of the precursor. The study provides detailed insights into how the composition of the synthesis solution affects the chemical evolution and micellar aggregation during formation of mesoporous silica. (C) 2018 Elsevier Inc. All rights reserved.

    Publikationen är tillgänglig i fulltext från 2020-03-13 13:33
  • 28.
    Boyd, Robert
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Söderlind, Fredrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Helmersson, Ulf
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Pilch, Iris
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Complex 3D nanocoral like structures formed by copper nanoparticle aggregation on nanostructured zinc oxide rods2016Ingår i: Materials letters (General ed.), ISSN 0167-577X, E-ISSN 1873-4979, Vol. 184, s. 127-130Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    This paper reports a new strategy for nanoparticle surface assembly so that they form anisotropic fibril like features, consisting of particles directly attached to each other, which can extend 500 nm from the surface. The particles are both formed and deposited in a single step process enabled via the use of a pulsed plasma based technique. Using this approach, we have successfully modified zinc oxide rods, up to several hundred nanometers in diameter, with 25 nm diameter copper nanoparticles for catalytic applications. The resulting structure could be modelled using a diffusion limited aggregation based approach. This gives the material the appearance of marine coral, hence the term nanocoral. (C) 2016 Elsevier B.V. All rights reserved.

  • 29.
    Calamba, Katherine
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Univ Lorraine, France.
    Jöesaar Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. SECO Tools AB, Sweden.
    Bruyere, S.
    Univ Lorraine, France.
    Pierson, J. F.
    Univ Lorraine, France.
    Boyd, Robert
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Andersson, J. M.
    SECO Tools AB, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    The effect of nitrogen vacancies on initial wear in arc deposited (Ti-0.52,Ti- Al-0.48)N-y, (y < 1) coatings during machining2019Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 358, s. 452-460Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Nitrogen deficient c-(Ti0.52Al0.48)Ny, y = 0.92, y = 0.87, and y = 0.75 coatings were prepared in different N-2/Ar discharges on WC-Co inserts by reactive cathodic arc deposition. The microstructure of the y = 0.92 coating show that spinodal decomposition has occurred resulting in the formation of coherent c-TiN- and c-AIN rich domains during cutting. The y = 0.87 and y = 0.75 coatings have exhibited a delay in decomposition due to the presence of nitrogen vacancies that lowers the free energy of the system. In the decomposed structure, grain boundaries and misfit dislocations enhance the diffusion of elements from the workpiece and the substrate (e.g. Fe, Cr, and Co) into the coatings and it becomes more susceptible to crater wear. The y = 0.87 sample displays the highest crater wear resistance because of its dense grain boundaries that prevent chemical wear. The y = 0.92 sample has the best flank wear resistance because the decomposition results in age hardening. The y = 0.75 sample contains the MAX-phase Ti(2)AIN after cutting. The chemical alteration within the y = 0.75 sample and its high amount of macroparticles cause its low wear resistance. The different microstructure evolution caused by different amount of N-vacancies result in distinctive interactions between chip and coating, which also causes difference in the initial wear mechanism of the (Ti,Al)/N-y coatings.

  • 30.
    Calamba, Katherine
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Univ Lorraine, France.
    Pierson, J. F.
    Univ Lorraine, France.
    Bruyere, S.
    Univ Lorraine, France.
    Le Febvrier, Arnaud
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Eklund, Per
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Barrirero, Jenifer
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Saarland Univ, Germany.
    Muecklich, F.
    Saarland Univ, Germany.
    Boyd, Robert
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Plasma och beläggningsfysik. Linköpings universitet, Tekniska fakulteten.
    Jöesaar Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. SECO Tools AB, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Dislocation structure and microstrain evolution during spinodal decomposition of reactive magnetron sputtered heteroepixatial c-(Ti-0.37,Al-0.63)N/c-TiN films grown on MgO(001) and (111) substrates2019Ingår i: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 125, nr 10, artikel-id 105301Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Heteroepitaxial c-(Ti-0.37,Al-0.63)N thin films were grown on MgO(001) and MgO(111) substrates using reactive magnetron sputtering. High resolution high-angle annular dark-field scanning transmission electron micrographs show coherency between the film and the substrate. In the as-deposited state, x-ray diffraction reciprocal space maps show a strained epitaxial film. Corresponding geometric phase analysis (GPA) deformation maps show a high stress in the film. At elevated temperature (900 degrees C), the films decompose to form iso-structural coherent c-Al- and c-TiN-rich domains, elongated along the elastically soft amp;lt;100amp;gt; directions. GPA analysis reveals that the c-TiN domains accommodate more dislocations than the c-AlN domains. This is because of the stronger directionality of the covalent bonds in c-AlN compared with c-TiN, making it more favorable for the dislocations to accumulate in c-TiN. The defect structure and strain generation in c-(Ti,Al)N during spinodal decomposition is affected by the chemical bonding state and elastic properties of the segregated domains.

  • 31.
    Calamba, Katherine
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. University of Lorraine, France.
    Schramm, Isabella
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Saarland University, Germany.
    Johansson Jöesaar, Mats P.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. SECO Tools AB, Sweden.
    Ghanbaja, J.
    University of Lorraine, France.
    Pierson, J. F.
    University of Lorraine, France.
    Mucklich, F.
    Saarland University, Germany.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Enhanced thermal stability and mechanical properties of nitrogen deficient titanium aluminum nitride (Ti0.54Al0.46Ny) thin films by tuning the applied negative bias voltage2017Ingår i: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 122, nr 6, artikel-id 065301Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Aspects on the phase stability and mechanical properties of nitrogen deficient (Ti0.54Al0.46)N-y alloys were investigated. Solid solution alloys of (Ti,Al)N were grown by cathodic arc deposition. The kinetic energy of the impinging ions was altered by varying the substrate bias voltage from -30V to -80 V. Films deposited with a high bias value of -80V showed larger lattice parameter, finer columnar structure, and higher compressive residual stress resulting in higher hardness than films biased at -30V when comparing their as-deposited states. At elevated temperatures, the presence of nitrogen vacancies and point defects (anti-sites and self-interstitials generated by the ion-bombardment during coating deposition) in (Ti0.54Al0.46)N-0.87 influence the driving force for phase separation. Highly biased nitrogen deficient films have point defects with higher stability during annealing, which cause a delay of the release of the stored lattice strain energy and then accelerates the decomposition tendencies to thermodynamically stable c-TiN and w-AlN. Low biased nitrogen deficient films have retarded phase transformation to w-AlN, which results in the prolongment of age hardening effect up to 1100 degrees C, i.e., the highest reported temperature for Ti-Al-N material system. Our study points out the role of vacancies and point defects in engineering thin films with enhanced thermal stability and mechanical properties for high temperature hard coating applications. Published by AIP Publishing.

  • 32.
    Chen, Yu-Hsiang
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Roa, J. J.
    Department of Materials Science and Metallurgical Engineering, Universitat Politècnica de Catalunya, Campus Diagonal Besòs-EEBE, 08019 Barcelona, Spain / Centre for Research in Multiscale Engineering of Barcelona, Universitat Politècnica de Catalunya, Campus Diagonal Besòs-EEBE, Barcelona, Spain.
    Chen, Yu-Hsiang
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Johansson-Jõesaar, Mats P.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Andersson, J. M.
    R&D Material and Technology Development, SECO Tools AB, SE-737 82 Fagersta, Sweden.
    Anglada, M. J.
    Department of Materials Science and Metallurgical Engineering, Universitat Politècnica de Catalunya, Campus Diagonal Besòs-EEBE, Barcelona, Spain / Centre for Research in Multiscale Engineering of Barcelona, Universitat Politècnica de Catalunya, Campus Diagonal Besòs-EEBE, Barcelona, Spain.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Rogström, Lina
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Enhanced thermal stability and fracture toughness of TiAlN coatings by Cr, Nb and V-alloying2018Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 342, s. 85-93Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The effect of metal alloying on mechanical properties including hardness and fracture toughness were investigated in three alloys, Ti 0.33Al0.50(Me) 0.17N (Me = Cr, Nb and V), and compared to Ti0.50Al0.50N, in the as-deposited state and after annealing. All studied alloys display similar as-deposited hardness while the hardness evolution during annealing is found to be connected to phase transformations, related to the alloy’s thermal stability. The most pronounced hardening was observed in Ti0.50Al0.50N, while all the coatings with additional metal elements sustain their hardness better and they are harder than Ti0.50Al0.50N after annealing at 1100 °C. Fracture toughness properties were extracted from scratch tests. In all tested conditions, as-deposited and annealed at 900 and 1100 °C, Ti0.33Al0.50Nb0.17N show the least surface and sub-surface damage when scratched despite the differences in decomposition behavior and h-AlN formation. Theoretically estimated ductility of phases existing in the coatings correlates well with their crack resistance. In summary, Ti0.33Al0.50Nb0.17N is the toughest alloy in both as-deposited and post-annealed states.

    Publikationen är tillgänglig i fulltext från 2020-02-17 16:38
  • 33.
    Chen, Yu-Hsiang
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Rongström, L.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Ostach, D.
    HZG, Germany.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Johansson-Jöesaar, Mats P
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. SECO Tools AB, Sweden.
    Schell, N.
    HZG, Germany.
    Birch, Jens
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Effects of decomposition route and microstructure on h-AlN formation rate in TiCrAlN alloys2017Ingår i: Journal of Alloys and Compounds, ISSN 0925-8388, E-ISSN 1873-4669, Vol. 691, s. 1024-1032Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The phase evolution of cubic (c), solid solution TixCr-0.37Al1-0.37-x N alloys with x = 0.03 and 0.16, and the kinetics of the hexagonal (h)-AlN formation are studied via in situ wide angle x-ray scattering experiments during high temperature (1000-1150 degrees C) annealing. Spinodal decomposition was observed in Ti0.16Cr0.36Al0.48N while Ti0.03Cr0.38Al0.59N decomposes through nucleation and growth of h-AlN, c-TiN and c-CrAlN. h-AlN is formed from c-CrAlN domains in both cases and the formation rate of h-AlN depends on the stability of the c-CrAlN domains. In Ti0.16Cr0.36Al0.48N, the c-CrAlN domains are stabilized by crystallographic coherency with the surrounding c-TiCrN in a microstructure originating from spinodal decomposition. This results in lower formation rates of h-AlN for this composition. These differences are reflected in higher activation energy for h-AlN formation in Ti0.16Cr0.36Al0.48N compared to Ti0.03Cr0.38Al0.59N. It also points out different stabilities of the intermediate phase c-CrAlN during phase decomposition of TiCrAlN alloys. Additional contributions to the low activation energy for formation of h-AlN in Ti0.03Cr0.38Al0.59N stems from precipitation at grain boundaries. (C) 2016 Elsevier B.V. All rights reserved.

  • 34.
    Chen, Yu-Hsiang
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Rogström, Lina
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Roa, JJ
    Departament de Ciència dels Materials i Enginyería Metal·lúrgica, Universitat Politècnica de Catalunya, EEBE-Campus Diagonal Besòs, Barcelona, Spain.
    Zhu, Jianqiang
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Schramm, Isabella
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten. Functional Materials, Department of Materials Science, Campus D3.3, Saarland University,Saarbrücken, Germany.
    Johnson, LJS
    Sandvik Coromant, SE-126 80 Stockholm, Sweden.
    Schell, N.
    Helmholtz-Zentrum Geesthacht (HZG), Geesthacht, Germany.
    Muecklich, F.
    Functional Materials, Department of Materials Science, Campus D3.3, Saarland University, Saarbrücken, Germany.
    Anglada, M. J.
    Departament de Ciència dels Materials i Enginyería Metal·lúrgica, Universitat Politècnica de Catalunya, EEBE-Campus Diagonal Besòs, Barcelona, Spain.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Thermal and mechanical stability of wurtzite-ZrA1N/cubic-TiN and wurtzite-ZrA1N/cubic-ZrN multilayers2017Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 324, s. 328-337Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The phase stability and mechanical properties of wurtzite (w)-Zr(0.25)A1(0.75)N/cubic (c)-TiN and w-Zr(0.25)A1(0.75)N/c-ZrN multilayers grown by arc evaporation are studied. Coherent interfaces with an orientation relation of c-TiN (111)[1-10]IIw-ZrAlN (0001)[11-20] form between ZrA1N and TiN sublayers during growth of the w-ZrAIN/c-TiN multilayer. During annealing at 1100 degrees C a c-Ti(Zr)N phase forms at interfaces between ZrA1N and TiN, which reduces the lattice mismatch so that the coherency and the compressive strain are partially retained, resulting in an increased hardness (32 GPa) after annealing. For the w-ZrAIN/c-ZrN multilayer, there is no coherency between sublayers leading to strain relaxation during annealing causing the hardness to drop. The retained coherency between layers and the compressive strain in the w-ZrAIN/c-TiN multilayer results in superior fracture toughness compared to the w-ZrAIN/c-ZrN multilayer as revealed by cross-sectional investigations of damage events under scratch and indentation tests. (C) 2017 Elsevier B.V. All rights reserved.

  • 35.
    Cordoba Gallego, Jose Manuel
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Ballem, Mohamed
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Johansson, Emma
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Growth of single crystalline dendritic Li(2)SiO(3) arrays from LiNO(3) and mesoporous SiO(2)2011Ingår i: Journal of Solid State Chemistry, ISSN 0022-4596, E-ISSN 1095-726X, Vol. 184, nr 7, s. 1735-1739Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    A solution based wet chemistry approach has been developed for synthesizing Li(2)SiO(3) using LiNO(3) and mesoporous silica as starting materials at 550 degrees C. A reaction path where NO and O(2) are formed as side-products is proposed. The crystals synthesized exhibit dendritic growth where the as-prepared nanodendrite is a typical 1-fold nanodendrite composed of one several microns long and some tenth of nanometers wide trunk with small branches, which are several hundreds of nanometers long and up to 70 nm in diameter. The effect of the structure of the mesoporous silica for the final morphology is discussed.

  • 36.
    Cordoba Gallego, Jose Manuel
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Growth and characterization of electroless deposited Cu films on carbon nanofibers2009Ingår i: SURFACE and COATINGS TECHNOLOGY, ISSN 0257-8972, Vol. 203, nr 22, s. 3459-3464Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Carbon nanofibers with two different microstructures, herringbone and platelet have been used as substrates to study the influence of electroless deposition parameters on the growth of Cu deposits. Flat glassy carbon and graphite powder substrates were also included in the study for comparison. Samples were analyzed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, FT-IR, and energy dispersive X-ray spectroscopy in terms of microstructure and chemical composition. The specific surface area was determined by sorption techniques. High quality copper films can be grown on carbon nanofibers at room temperature if carbon nanofibers pretreatment is properly adjusted. The optimized process is easily up scaled to larger batches of carbon nanofibers.

  • 37.
    Cordoba Gallego, Jose Manuel
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Tamayo-Ariztondo, J
    Tecnun University Navarra.
    Molina-Aldareguia, J M
    Fdn IMDEA Mat.
    Elizalde, M R
    Tecnun University Navarra.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Morphology influence of the oxidation kinetics of carbon nanofibers2009Ingår i: CORROSION SCIENCE, ISSN 0010-938X, Vol. 51, nr 4, s. 926-930Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    This paper reports the stability and oxidation rate of five types of carbon nanofiber (CNF) with distinctly different orientation of their graphite sheets based on conversion to CO2 when heated in the presence of oxygen. A non-isothermal technique was used to determine the oxidation kinetic parameters including the activation energy (E-a) Graphite shows a similar activation energy (E-a = 158 kJ/mol(-1)) to CNF with longitudinal alignment (E-a = 156kJ/mol(-1)). CNF type herringbone (E-a = 126kJ/mol(-1)) and platelet (E-a = 145 kJ/mol(-1)) show the lowest oxidation resistance which improved dramatically after a heat treatment at 3023 K of the herringbone (E-a = 216 kJ/mol(-1)) and platelet (E-a = 174 kJ/mol(-1)) structures.

  • 38.
    Dalibon, Eugenia. L.
    et al.
    UTN, Argentina.
    Czerwiec, Thierry
    Univ Lorraine, France.
    Trava-Airoldi, Vladimir J.
    INPE, Brazil.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Rogström, Lina
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Bruhl, Sonia P.
    UTN, Argentina.
    Characterization of DLC coatings over nitrided stainless steel with and without nitriding pre-treatment using annealing cycles2019Ingår i: JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY-JMRandT, ISSN 2238-7854, Vol. 8, nr 2, s. 1653-1662Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Amorphous hydrogenated diamond-like carbon (DLC) coatings were deposited using plasma assisted chemical vapour deposition (PACVD) on precipitation hardening (PH) stainless steel.Plasma nitriding has been used as pre-treatment to enhance adhesion and mechanical properties. Chemical and mechanical properties of DLC coatings are dependent on the hydrogen content and so on the relation between sp(3)/sp(2) bondings. The bondings and the structure of the DLC film change with temperature. In this work, a study of the thermal degradation and the evolution of the mechanical properties of DLC coatings over PH stainless steel have been carried out, including the effect of an additional nitrided layer. Nitrided and non-nitrided steel samples were subjected to the same coated in the same conditions, and they were submitted to the same thermal cycles, heating from room temperature to 600 degrees C in several steps. After each cycle, Raman spectra and surface topography measurements were performed and analyzed. Nanohardness measurements and tribological tests, using a pin-on-disc machine, were carried out to analyze variations in the friction coefficient and the wear resistance. The duplex sample, with nitriding as pre-treatment showed a better thermal stability. For duplex sample, the coating properties, such as adhesion, and friction coefficient were sustained after annealing at higher temperatures; whereas it was not the case for only coated sample. (C) 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda.

  • 39.
    Dalibon, Eugenia L.
    et al.
    University of Tecnol Nacl UTN FRCU, Argentina.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Rogström, Lina
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Trava-Airoldi, Vladimir J.
    INPE, Brazil.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Bruhl, Sonia P.
    University of Tecnol Nacl UTN FRCU, Argentina.
    Carbon Based Coatings Deposited on Nitrided Stainless Steel: Study of Thermal Degradation2017Ingår i: PROCEEDINGS OF THE 3RD PAN AMERICAN MATERIALS CONGRESS, SPRINGER INTERNATIONAL PUBLISHING AG , 2017, s. 57-66Konferensbidrag (Refereegranskat)
    Abstract [en]

    Amorphous hydrogenated carbon (DLC) coatings have a high hardness depending on the relative amount of sp(3)/sp(2) bondings. They also exhibit an extremely low friction coefficient and are chemically inert. However, these coatings have some disadvantages which limit their applications. For instance, adhesion is poor when they are deposited on metallic substrates and they are also unstable at high temperatures, degrading into graphite and loosing hardness. In this work, DLC coatings were deposited on precipitation hardening stainless steel (PH Corrax) which was plasma nitrided before the coating deposition. The samples were submitted to annealing treatments for an hour at different temperatures from 200 to 600 degrees C, together with a control group, which was only coated but not nitrided. After each annealing cycle, Raman Spectroscopy, nanoindentation and microscopy were used to check film properties. It was demonstrated that the nitriding pre treatment improved not only adhesion but also the thermal stability of the DLC, slowing degradation and preventing delamination.

  • 40.
    Engberg, David L. J.
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Johnson, Lars J. S.
    Sandvik Coromant, Stockholm, Sweden.
    Johansson-­‐Jöesaar, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi. Linköpings universitet, Tekniska fakulteten. SECO Tools AB, Fagersta, Sweden.
    Lu, Jun
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    Thuvander, Mattias
    Department of Applied Physics, Chalmers University of Technology, Göteborg, Sweden.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Solid Solution and Segregation Effects in Arc-Deposited Ti1-xSixN Thin Films Resolved on the nanometer scale by 15N Isotopic Substitution in AtomP robe TomographyManuskript (preprint) (Övrigt vetenskapligt)
    Abstract [en]

    Nanostructured TiSiN is an important material in wear--‐resistant coatings for extending the lifetime of cutting tools. Yet, the understanding regarding the structure, phase composition, and bonding on the detailed nanometer scale, which determines the properties of TiSiN, is lacking. This limits our understanding of the growth phenomena and eventually a larger exploitation of the material. By substituting natN2 with 15N2 during reactive arc deposition of TiSiN thin films, atom probe tomography (APT) gives elemental sensitivity and sub-nanometer resolution, a finer scale than what can be obtained by commonly employed energy dispersive electron spectroscopy in scanning transmission electron microscopy. Using a combination of analytical transmission electron microscopy and APT we show that arc-deposited Ti0.92Si0.0815N and Ti0.81Si0.1915N exhibit Si segregation on the nanometer scale in the alloy films. APT composition maps and proximity histograms from domains with higher than average Ti content show that the TiN domains contain at least ~2 at. % Si for Ti0.92Si0.08N and ~5 at. % Si for Ti0.81Si0.19N, thus confirming the formation of solid solutions. The formation of relatively pure SiNy domains in the Ti0.81Si0.19N films is tied to pockets between microstructured, columnar features in the film. Finer SiNy enrichments seen in APT possibly correspond to tissue layers around TiN crystallites, thus effectively hindering growth of TiN crystallites, causing TiN renucleation and thus explaining the featherlike nanostructure within the columns of these films. For the stoichiometry of the TiN phase, we establish a global under stoichiometry, in accordance with the tendency for SiNy films to have tetrahedral bonding coordination towards a nominal Si3N4 composition.

  • 41.
    Eriksson, Anders
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Jensen, Jens
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Näslund, Lars-Åke
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Sjölen, J.
    Seco Tools AB, Fagersta, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Rosén, Johanna
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Arc deposition of Ti–Si–C–N thin films from binary and ternary cathodes — Comparing sources of C2012Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 213, s. 145-154Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Ti–Si–C–N thin films with composition of 1–11 at.% Si and 1–20 at.% C have been deposited onto cemented carbide substrates by arcing Ti–Si cathodes in a CH4 + N2 gas mixture and, alternatively, through arcing Ti–Si–C cathodes in N2. Films of comparable compositions from the two types of cathodes have similar structure and properties. Hence, C can be supplied as either plasma ions generated from the cathode or atoms from the gas phase with small influence on the structural evolution. Over the compositional range obtained, the films were dense and cubic-phase nanocrystalline, as characterized by X-ray diffraction, ion beam analysis, and scanning and transmission electron microscopy. The films have high hardness (30–40 GPa by nanoindentation) due to hardening from low-angle grain boundaries on the nanometer scale and lattice defects such as growth-induced vacancies and alloying element interstitials.

  • 42.
    Eriksson, Anders
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Zhu, Jianqiang
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Jensen, Jens
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Greczynski, Grzegorz
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan. Seco Tools AB, Sweden.
    Sjölen, Jacob
    Seco Tools AB, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Rosén, Johanna
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Ti-Si-C-N Thin Films Grown by Reactive Arc Evaporation from Ti3SiC2 Cathodes2011Ingår i: Journal of Materials Research, ISSN 0884-2914, E-ISSN 2044-5326, Vol. 26, s. 874-881Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Ti-Si-C-N thin films were deposited onto WC-Co substrates by industrial scale arc evaporation from Ti3SiC2 compound cathodes in N2 gas. Microstructure and hardness were found to be highly dependent on the wide range of film compositions attained, comprising up to 12 at.% Si and 16 at.% C. Nonreactive deposition yielded films consisting of understoichiometric TiCx, Ti and silicide phases with high (27 GPa) hardness. At a nitrogen pressure of 0.25-0.5 Pa, below that required for N saturation, superhard, 45-50 GPa, (Ti,Si)(C,N) films with a nanocrystalline feathered structure were formed. Films grown above 2 Pa displayed crystalline phases of more pronounced nitride character, but with C and Si segregated to grain boundaries to form weak grain boundary phases. In abundance of N, the combined presence of Si and C disturb cubic phase growth severely and compromises the mechanical strength of the films.

  • 43.
    Eriksson, Anders
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Zhu, Jianqiang
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan. Seco Tools AB, Sweden.
    Sjölen, Jacob
    Seco Tools AB, Sweden.
    Jensen, Jens
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Rosén, Johanna
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Layer Formation by Resputtering in Ti-Si-C Hard Coatings during Large Scale Cathodic Arc Deposition2011Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 205, nr 15, s. 3923-3930Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    This paper presents the physical mechanism behind the phenomenon of self-layering in thin films made by industrial scale cathodic arc deposition systems using compound cathodes and rotating substrate fixture. For Ti-Si-C films, electron microscopy and energy dispersive x-ray spectrometry reveals a trapezoid modulation in Si content in the substrate normal direction, with a period of 4 to 23 nm dependent on cathode configuration. This is caused by preferential resputtering of Si by the energetic deposition flux incident at high incidence angles when the substrates are facing away from the cathodes. The Ti-rich sub-layers exhibit TiC grains with size up to 5 nm, while layers with high Si-content are less crystalline. The nanoindentation hardness of the films increases with decreasing layer thickness.

  • 44.
    Escalera, E.
    et al.
    Luleå University of Technology, Sweden; San Simon University, Bolivia.
    Garcia, G.
    Luleå University of Technology, Sweden.
    Teran, R.
    San Simon University, Bolivia.
    Tegman, R.
    Luleå University of Technology, Sweden.
    Antti, M-L.
    Luleå University of Technology, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska fakulteten.
    The production of porous brick material from diatomaceous earth and Brazil nut shell ash2015Ingår i: Construction and Building Materials, ISSN 0950-0618, E-ISSN 1879-0526, Vol. 98, s. 257-264Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Diatomaceous earth was mixed with Brazil nut shell ash (BNS ash) in different amounts between 0 and 30 wt% and sintered at temperatures between 750 and 950 degrees C. The BNS ash contains 33 wt% K2O and 11 wt% CaO mainly in carbonate form. The addition of BNS ash into the diatomaceous earth caused significant changes of the microstructure after sintering. The BNS ash addition produces lightweight porous bricks with acceptable strength at lower sintering temperature. The best combination of strength and porosity was achieved for a mixture of 10 wt% of BNS ash in the diatomaceous earth sintered at 850 degrees C. The achieved high porosity was 49%, density 1.06 g/cm(3), thermal conductivity 0.20 W/(m K) and the compressive strength was 8.5 MPa. (C) 2015 Elsevier Ltd. All rights reserved.

  • 45.
    Escalera, Edwin
    et al.
    Division of Materials Science, Luleå University of Technology.
    Antti, M.
    Division of Materials Science, Luleå University of Technology.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Thermal treatment and phase formation in kaolinite and illite based clays from tropical regions of Bolivia2012Konferensbidrag (Refereegranskat)
    Abstract [en]

    The aim of this study was to compare the thermal behaviour of clays containing illite and kaolinite in various proportions. The clays contained small amounts of K and Fe, which act as fluxing agents. In order to investigate the phase formations during heating, the samples were examined in a differential scanning calorimeter at temperatures up to 1300°C. The thermal expansion of the samples was determined by dilatometer measurements from room temperature up to 1150°C. Phases were identified using x-ray diffraction and scanning electron microscopy.

    In all samples, most of the kaolinite was transformed into metakaolinite during heating up to 650°C, while illite remained unchanged up to 950°C. There was no influence of K and Fe on dehydroxylation. Metakaolinite formed at temperatures above 950°C leading to a Si-Al spinel. Furthermore, mullite was formed in the temperature interval 1050-1150°C. In this temperature range, the mechanism of mullite formation depended on the amount of K and Fe in the samples, changing the temperature of formation of mullite. It was observed by x-ray diffraction that most of the illite was transformed into a Si-Al spinel phase at 1050°C, and during further heating transformed into mullite. An increased amount of illite in the clays slightly decreased the melting temperature. The dilatometer measurements showed expansion and shrinkage for the dehydroxylation and spinel-phase formation, respectively.

  • 46.
    Escalera, Edwin
    et al.
    Division of Engineering Materials, Department of Applied Physics and Mechanical Engineering, Luleå University of Technology, Luleå, Sweden..
    Ballem, Mohamed A.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Cordoba, José M.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Antti, Marta-Lena
    Division of Engineering Materials, Department of Applied Physics and Mechanical Engineering, Luleå University of Technology, Luleå, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Synthesis of homogeneously dispersed cobalt nanoparticles in the pores of functionalized SBA-15 silica2012Ingår i: Powder Technology, ISSN 0032-5910, E-ISSN 1873-328X, Vol. 221, nr S1, s. 359-364Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Cobalt nanoparticles were prepared at room temperature by reducing cobalt sulfate heptahydrate with sodium borohydride and using functionalized SBA-15 mesoporous silica as a hard template. It was found that both external and internal fuctionalization of silica walls play a crucial role on the infiltration and reaction of the reagents in the silica framework. Subsequent heat treatment of the impregnated silica at 500 °C in air or nitrogen atmospheres leads to growth of crystals of the deposited cobalt and formation of cobalt and cobalt oxide nanoparticles, respectively. Dissolution of the silica template by NaOH resulted in well dispersed Co and Co3O4 nanoparticles ranging in size from 2 to 4 nm. The functionalization of the silica was studied by FTIR, N2-physisorption, and thermogravimetric techniques and the obtained nanoparticles were characterized by XRD, TEM and EDX analysis.

  • 47.
    Escalera, Edwin
    et al.
    Luleå University of Technology, Sweden; San Simon University, Bolivia.
    Tegman, Ragnar
    Luleå University of Technology, Sweden.
    Antti, Marta-Lena
    Luleå University of Technology, Sweden.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    High temperature phase evolution of Bolivian kaolinitic-illitic clays heated to 1250 degrees C2014Ingår i: Applied Clay Science, ISSN 0169-1317, E-ISSN 1872-9053, Vol. 101, s. 100-105Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The thermal behaviour of two types of clays collected from different locations in Bolivia has been studied. The clays contain kaolinite, illite, quartz and small amounts of microcline. The phase evolutions have been characterized from room temperature to 1250 degrees C. For both clays, kaolinite is completely transformed into metakaolinite when heated up to 650 degrees C. During further heating to 1050 degrees C, illite undergoes total dehydroxylation. Mullite is formed in the temperature interval of 1050-1150 degrees C and its formation rate is dependent on the amount of K and Fe present in the clays. The clay with higher amounts of K (3.2 mass %) and Fe (5.6 mass%) has an onset temperature for sintering at about 900 degrees C and an onset temperature for liquid formation at 1080 degrees C. This is about 50 degrees C lower onset temperature for sintering and 94 degrees C lower onset temperature for liquid formation when compared with the clay with lower amounts of K (2.3 mass %) and Fe (1.6 mass %).

  • 48.
    Fager, Hanna
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Andersson, J. M.
    Seco Tools AB, SE-737 82 Fagersta, Sweden.
    Johansson, Mats
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Hultman, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska högskolan.
    Growth of Hard Amorphous Ti-Al-Si-N Thin Films by Cathodic Arc Evaporation2013Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 235, nr 25, s. 376-385Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Ti(1−x−y)AlxSiyNz (0.02≤x≤0.46, 0.02≤y≤0.28, and 1.08≤z≤1.29) thin films were grown on cemented carbide substrates in an industrial scale cathodic arc evaporation system using Ti-Al-Si compound cathodes in a N2 atmosphere. The microstructure of the as-deposited films changes from nanocrystalline to amorphous by addition of Al and Si to TiN. Upon incorporation of 12 at% Si and 18 at% Al, the films assume an x-ray amorphous state. Post-deposition anneals show that the films are thermally stable up to 900 ◦C. The films exhibit age hardening up to 1000 ◦C with an increase in hardness from 21.9 GPa for as-deposited films to 31.6 GPa at 1000 ◦C. At 1100 ◦C severe out-diffusion of Co and W from the substrate occur, and the films recrystallize into c-TiN and w-AlN.

  • 49.
    Forsén, Rikard
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Coherency strain engineered decomposition of unstable multilayer alloys for improved thermal stability2013Ingår i: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 114, nr 24, s. 244303-Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    A concept to improve hardness and thermal stability of unstable multilayer alloys is presented based on control of the coherency strain such that the driving force for decomposition is favorably altered. Cathodic arc evaporated cubic TiCrAlN/Ti 1−x Cr x N multilayer coatings are used as demonstrators. Upon annealing, the coatings undergo spinodal decomposition into nanometer-sized coherent Ti- and Al-rich cubic domains which is affected by the coherency strain. In addition, the growth of the domains is restricted by the surrounding TiCrN layer compared to a non-layered TiCrAlN coating which together results in an improved thermal stability of the cubic structure. A significant hardness increase is seen during decomposition for the case with high coherency strain while a low coherency strain results in a hardness decrease for high annealing temperatures. The metal diffusion paths during the domain coarsening are affected by strain which in turn is controlled by the Cr-content (x) in the Ti 1−x Cr x N layers. For x = 0 the diffusion occurs both parallel and perpendicular to the growth direction but for x > =0.9 the diffusion occurs predominantly parallel to the growth direction. Altogether this study shows a structural tool to alter and fine-tune high temperature properties of multicomponent materials.

  • 50.
    Forsén, Rikard
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Johansson, M P.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Odén, Magnus
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Ghafoor, Naureen
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Nanostrukturerade material. Linköpings universitet, Tekniska högskolan.
    Effects of Ti alloying of AlCrN coatings on thermal stability and oxidation resistance2013Ingår i: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 534, s. 394-402Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Quaternary cubic (TixCr1 − xAl~ 0.60)1 N1 coatings with 0 < x < 0.33 have been grown using reactive cathodic arc evaporation. When adding Ti the hardness was retained after annealing up to 1100 °C which is a dramatic improvement compared to CrAlN coatings. The coatings showed an age hardening process caused by spinodal decomposition into coherent TiCr- and Al-rich cubic TiCrAlN domains and the formation of hexagonal AlN precipitates and cubic TiCrN domains in the vicinity of the grain boundaries. The improved hardness was attributed to the stabilization of the cubic structure suppressing the formation and growth of hexagonal AlN. Furthermore, the presence of Ti atoms generated incoherent nanometer-sized crystallites within the hexagonal AlN precipitates disrupting the hexagonal lattice during the coarsening process.

    The addition of Ti promoted the formation of a TiO2 layer over Al2O3 resulting in a lower oxidation resistance. However, by tuning the composition it is possible to design coatings to have both good oxidation resistance and good high temperature mechanical stability.

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