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von Fieandt, L., Larsson, T., Boman, M. & Lindahl, E. (2019). Texture formation in chemical vapor deposition of Ti(C,N). Journal of Crystal Growth, 508, 90-95
Open this publication in new window or tab >>Texture formation in chemical vapor deposition of Ti(C,N)
2019 (English)In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 508, p. 90-95Article in journal (Refereed) Published
Abstract [en]

The growth mechanism of Ti(C,N) coatings produced by chemical vapor deposition was investigated as a function of the TiCl4/CH3CN molar ratio in excess of H-2. The depositions were carried out at a total pressure of 8 kPa, using single crystalline (0 0 l) alpha-Al2O3 substrates. The Ti(C,N) coatings were characterized by X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. The investigated coatings were between 6 and 13 mu m thick. The reaction orders of TiCl4 CH3CN were determined to 0 and 1, respectively, showing that CH3CN is the rate-determining reactant. The preferred orientation of the deposited Ti(C,N) was investigated, showing that molar ratios TiCl4 /CH3CN higher than 2.5 lead to < 2 1 1 >/< 3 1 1 > oriented coatings. A formation mechanism for the < 2 1 1 >/< 3 1 1 > orientations is suggested. Such high ratios lead to the formation of Ti {1 1 1} twinning planes, which provide surface sites that can facilitate fast dissociation of the strong cyanide bond, and thereby cause faster growth in the < 2 1 1 >/< 3 1 1 > directions. Coatings deposited at lower molar ratios show a pronounced < 1 1 1 > out-of-plane orientation, characterized by a {1 1 1} rocking curve yielding values for full width at half maximum (FWHM) below 0.5 degrees.

Place, publisher, year, edition, pages
Elsevier, 2019
Keywords
Growth model, Titanium compounds, Chemical vapor deposition process, X-ray diffraction
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-376714 (URN)10.1016/j.jcrysgro.2018.12.030 (DOI)000456430200012 ()
Funder
Swedish Foundation for Strategic Research , RIF14-0053Swedish Foundation for Strategic Research , RMA15-0048Swedish Research Council, C0514401
Available from: 2019-02-12 Created: 2019-02-12 Last updated: 2019-02-12Bibliographically approved
Kjellander, M., Billinger, E., Ramachandraiah, H., Boman, M., Bergström Lind, S. & Johansson, G. (2018). A flow-through nanoporous alumina trypsin bioreactor for mass spectrometry peptide fingerprinting. Journal of Proteomics, 172, 165-172
Open this publication in new window or tab >>A flow-through nanoporous alumina trypsin bioreactor for mass spectrometry peptide fingerprinting
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2018 (English)In: Journal of Proteomics, ISSN 1874-3919, E-ISSN 1876-7737, Vol. 172, p. 165-172Article in journal (Refereed) Published
Abstract [en]

Mass spectrometry-based proteomics benefits from efficient digestion of protein samples. In this study, trypsinwas immobilized on nanoporous anodized alumina membranes to create an enzyme reactor suitable for peptidemassfingerprinting. The membranes were derivatized with 3-aminopropyltriethoxysilane and the amino groupswere activated with carbonyldiimidazole to allow coupling of porcine trypsin viaε-amino groups. The functionwas assessed using the artificial substrate Nα-Benzoyl-L-arginine 4-nitroanilide hydrochloride, bovine ribonu-clease A and a human plasma sample. A 10-membraneflow-through reactor was used for fragmentation and MSanalysis after a single pass of substrate both by collection of product and subsequent off-line analysis, and bycoupling on-line to the instrument. The peptide pattern allowed correct identification of the single target proteinin both cases, and of > 70 plasma proteins in single pass mode followed by LC-MS analysis. The reactor retained76% of the initial activity after 14 days of storage and repeated use at room temperature.

Significance:This manuscript describes the design of a stable enzyme reactor that allows efficient and fast di-gestion with negligible leakage of enzyme and enzyme fragments. The high stability facilitates the use in anonline-setup with MS detection since it allows the processing of multiple samples within an extended period of time without replacement.

Keywords
nanoporous aluminum oxide, immobilization, trypsin, peptide mass fingerprinting, enzyme stability
National Category
Biochemistry and Molecular Biology Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-210118 (URN)10.1016/j.jprot.2017.09.008 (DOI)000423655300016 ()28942014 (PubMedID)
Funder
Swedish Research Council, 2005-3308Magnus Bergvall Foundation, 2015-01200Åke Wiberg Foundation, M14-0127Carl Tryggers foundation , CST 15:57Magnus Bergvall Foundation, 201601675
Available from: 2013-10-31 Created: 2013-10-31 Last updated: 2018-03-29Bibliographically approved
von Fieandt, L., Larsson, T., Lindahl, E., Bäcke, O. & Boman, M. (2018). Chemical vapor deposition of TiN on transition metal substrates. Surface & Coatings Technology, 334, 373-383
Open this publication in new window or tab >>Chemical vapor deposition of TiN on transition metal substrates
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2018 (English)In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 334, p. 373-383Article in journal (Refereed) Published
Abstract [en]

The growth of chemical vapor deposited TiN from a reaction gas mixture of TiCl4, N-2 and H-2 was investigated on three different transition metal substrates: Fe, Co and Ni at deposition temperatures ranging from 850 degrees C to 950 degrees C. The interactions between the substrate metals and the gas phase were investigated using thermodynamic calculations. The TiN coatings were characterized by scanning electron microscopy, scanning transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy and transmission Kikuchi diffraction. Chemical vapor deposition (CVD) of TiN on Co substrates resulted in dense, columnar coatings of single phase TiN. The activation energy for TiN deposition on Co was determined to be 90 kJ/mol. CVD of TiN on Fe substrates caused severe substrate corrosion by the formation of gaseous FeClx. Due to the substrate corrosion, the activation energy could not be determined. Furthermore, it was found that CVD of TiN on Ni substrates produced a phase mixture of TiN and Ni3Ti. Formation of Ni3Ti could be minimized by decreasing the H-2 partial pressure and increasing the N-2 partial pressure. Deposition on Ni yielded two different activation energies, 40 kJ/mol in the temperature interval 850 degrees C to 900 degrees C and 165 kJ/mol in the interval 900 degrees C to 950 degrees C. This is an indication of two different types of process control, which were identified as Ni diffusion into the growing film and a gas phase processes. The results of the present study showed that CVD of TiN on a cemented carbide using Fe and Ni in the binder phase, must be optimized in order to avoid corrosion or unwanted phases. Methods to achieve this are presented in this paper.

Place, publisher, year, edition, pages
Elsevier, 2018
Keywords
CVD, TiN, Alternate binder phase, Thermodynamic calculations
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-335908 (URN)10.1016/j.surfcoat.2017.11.063 (DOI)000423894700045 ()
Funder
Swedish Foundation for Strategic Research , RMA15-0048
Available from: 2017-12-10 Created: 2017-12-10 Last updated: 2018-04-04Bibliographically approved
Hedin, A., Johansson, A. J., Lilja, C., Boman, M., Berastegui, P., Berger, R. & Ottosson, M. (2018). Corrosion of copper in pure O2-free water?. Corrosion Science, 137, 1-12
Open this publication in new window or tab >>Corrosion of copper in pure O2-free water?
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2018 (English)In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 137, p. 1-12Article in journal (Refereed) Published
Abstract [en]

Copper exposed to pure, O-2-free water for several months in glass- and metal-contained, well-controlled systems shows no evidence of corrosion, either through hydrogen evolution or through the occurrence of oxidized copper. The results contradict the interpretation of recent experiments where it has been claimed that copper corrodes in pure, O-2-free water far above the very limited extent predicted by established thermodynamic data. Reasons for the different experimental outcomes are discussed. Experimental and theoretical efforts to identify hitherto unknown, potentially corrosion driving species of the Cu-O-H system and studies of copper/water surface reactions are reviewed as background for the present study.

Keywords
Copper, Corrosion, Water, Hydrogen
National Category
Corrosion Engineering
Identifiers
urn:nbn:se:uu:diva-387458 (URN)10.1016/j.corsci.2018.02.008 (DOI)000436213400001 ()
Available from: 2019-06-25 Created: 2019-06-25 Last updated: 2019-06-25Bibliographically approved
von Fieandt, L., Johansson, K., Lindahl, E., Larsson, T., Boman, M. & Rehnlund, D. (2018). Corrosion properties of CVD grown Ti(C,N) coatings in 3.5 wt-% NaCl environment. Corrosion Engineering, Science and Technology, 53(4), 316-320
Open this publication in new window or tab >>Corrosion properties of CVD grown Ti(C,N) coatings in 3.5 wt-% NaCl environment
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2018 (English)In: Corrosion Engineering, Science and Technology, ISSN 1478-422X, E-ISSN 1743-2782, Vol. 53, no 4, p. 316-320Article in journal (Refereed) Published
Abstract [en]

The corrosion behaviour of Titanium carbonitride (Ti(C,N)) films grown by chemical vapour deposition was analysed in artificial sea water environment. From potentiodynamic polarisation curves, two passivation zones were detected, which originated from an initial oxidation of TiC and TiN to TiO2 followed by growth of the TiO2 layer upon increased polarisation. X-ray photoelectron spectroscopy analyses verified the mechanism by detecting a gradual decrease in Ti(C,N) peaks accompanied by a gradual increase of oxidised Ti (e.g. TiO2). It was likewise found that carbon in TiC mainly decomposes into carbonate species while the nitrogen in TiN remains elemental and likely escapes as nitrogen gas. Accordingly, Ti(C,N) behaves like a superposition of TiC and TiN with their individual oxidation behaviour, resulting in a highly corrosion resistant material.

Keywords
Corrosion, Ti(C, N), CVD, XPS
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-355699 (URN)10.1080/1478422X.2018.1467150 (DOI)000431534000010 ()
Funder
Swedish Foundation for Strategic Research , RMA15-0048]
Available from: 2018-07-04 Created: 2018-07-04 Last updated: 2018-07-04Bibliographically approved
von Fieandt, L., Johansson, K., Larsson, T., Boman, M. & Lindahl, E. (2018). On the growth, orientation and hardness of chemical vapor deposited Ti(C,N). Thin Solid Films, 645, 19-26
Open this publication in new window or tab >>On the growth, orientation and hardness of chemical vapor deposited Ti(C,N)
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2018 (English)In: Thin Solid Films, ISSN 0040-6090, E-ISSN 1879-2731, Vol. 645, p. 19-26Article in journal (Refereed) Published
Abstract [en]

Chemical vapor deposition (CVD) of Ti(C,N) from a reaction gas mixture of TiCl4, CH3CN, H2 and N2 was investigated with respect to gas phase composition and kinetics. The gas phase composition was modelled by thermodynamic calculations and the growth rate of the CVD process was measured when replacing H2 for N2 while the sum of partial pressures H2+N2 was kept constant. The N2/H2 molar ratio was varied from 0 to 19. Single crystal c-sapphire was used as substrates. It was found that low molar ratios (N2/H2 molar ratio below 0.6) lead to an increased Ti(C,N) growth rate with up to 22%, compared to deposition without added N2. The mechanism responsible for the increased growth rate was attributed to the formation and increased gas phase concentration of one major growth species, HCN, in the gas phase. The texture of the Ti(C,N) films were also studied. ⟨211⟩ textured layers were deposited at N2/H2 molar ratios below 9. At higher molar ratios, ⟨111⟩ oriented Ti(C,N) layers were deposited and the grain size increased considerably. The films deposited at a N2/H2 ratio above 9 exhibited superior hardness, reaching 37GPa. The increased hardness is attributed to an almost epitaxial orientation between the layer and the substrate. The absence of grain twinning in the ⟨111⟩ oriented layer also contributed to the increased hardness.The Ti(C,N) layers were characterized by elastic recoil detection analysis, X-ray photo electron spectroscopy, scanning electron microscopy, X-ray diffraction and nanoindentation.

Keywords
CVD, Ti(C, N), Hard coating, Thermodynamic modelling
National Category
Materials Chemistry
Research subject
Chemistry with specialization in Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-334644 (URN)10.1016/j.tsf.2017.10.037 (DOI)000418305200004 ()
Funder
Swedish Foundation for Strategic Research , RMA15-0048Swedish Foundation for Strategic Research , RIF14-0053Swedish Research Council, C0514401
Available from: 2017-11-24 Created: 2017-11-24 Last updated: 2018-01-25Bibliographically approved
Ottosson, M., Boman, M., Berastegui, P., Andersson, Y., Hahlin, M., Korvela, M. & Berger, R. (2018). Response to the comments by P. Szakalos, T. angstrom kermark and C. Leygraf on the paper "Copper in ultrapure water, a scientific issue under debate" [Letter to the editor]. Corrosion Science, 142, 308-311
Open this publication in new window or tab >>Response to the comments by P. Szakalos, T. angstrom kermark and C. Leygraf on the paper "Copper in ultrapure water, a scientific issue under debate"
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2018 (English)In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 142, p. 308-311Article in journal, Letter (Other academic) Published
Keywords
Copper, XPS, AES, Oxidation
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:uu:diva-366387 (URN)10.1016/j.corsci.2018.02.003 (DOI)000444933400030 ()
Available from: 2018-11-21 Created: 2018-11-21 Last updated: 2018-11-21Bibliographically approved
Fondell, M., Gorgoi, M., Boman, M. & Lindblad, A. (2018). Surface modification of iron oxides by ion bombardment – comparing depth profiling by HAXPES and Ar ion sputtering. Journal of Electron Spectroscopy and Related Phenomena, 224, 23-26
Open this publication in new window or tab >>Surface modification of iron oxides by ion bombardment – comparing depth profiling by HAXPES and Ar ion sputtering
2018 (English)In: Journal of Electron Spectroscopy and Related Phenomena, ISSN 0368-2048, E-ISSN 1873-2526, Vol. 224, p. 23-26Article in journal (Refereed) Published
Abstract [en]

Iron oxide in the form of maghemite  γ-Fe2O3  and hematite α-Fe2O3 has been studied with x-ray photoelectron spectroscopy. It is found that even low energy sputtering induces a reduction of the surface layer into FeO. Satellites in the Fe 2p  core level spectra are used to determine the oxidation state of iron. Depth profiling with changing photon energy shows that the unsputtered films are homogeneous and that the information obtained from sputtering thus, in this instance, represents sputter damages to the sample.

Place, publisher, year, edition, pages
Elsevier, 2018
Keywords
Hard X-ray Photoelectron Spectroscopy, Depth profiling, Iron oxide, HAXPES, synchrotron radiation
National Category
Materials Engineering Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-232947 (URN)10.1016/j.elspec.2017.09.008 (DOI)000428825400005 ()
Funder
EU, FP7, Seventh Framework Programme, 312284The Royal Swedish Academy of SciencesSwedish Research Council, 2014-6463
Available from: 2014-09-28 Created: 2014-09-28 Last updated: 2018-06-05Bibliographically approved
von Fieandt, L., Fallqvist, M., Larsson, T., Lindahl, E. & Boman, M. (2018). Tribological properties of highly oriented Ti(C,N) deposited by chemical vapor deposition. Tribology International, 119, 593-599
Open this publication in new window or tab >>Tribological properties of highly oriented Ti(C,N) deposited by chemical vapor deposition
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2018 (English)In: Tribology International, ISSN 0301-679X, E-ISSN 1879-2464, Vol. 119, p. 593-599Article in journal (Refereed) Published
Abstract [en]

Two Ti(C,N) coatings were tested by means of micro abrasion and scratch testing. The coatings differed in grain size, orientation (<111> and <111>, <311> and <211> respectively) and hardness (36 GPa and 23 GPa respectively). The <111> oriented coating had a 20% higher wear resistance compared to the reference coating when abraded with 1 pm diamonds. When abraded with 6 pm diamonds the abrasion resistance of the reference coating was superior compared to the <111> oriented coating by 36%. Furthermore, it was found that the <111> oriented coating had 35% better adhesion compared to the reference. The improved mechanical properties of the <111> oriented coating was attributed to a high degree of orientation and the higher hardness.

National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-335909 (URN)10.1016/j.triboint.2017.11.040 (DOI)000424960500056 ()
Funder
Swedish Foundation for Strategic Research , RMA15-0048
Available from: 2017-12-10 Created: 2017-12-10 Last updated: 2018-04-06Bibliographically approved
Ottosson, M., Boman, M., Berastegui, P., Andersson, Y., Hedlund, M., Korvela, M. & Berger, R. (2017). Copper in ultrapure water, a scientific issue under debate. Corrosion Science, 122, 53-60
Open this publication in new window or tab >>Copper in ultrapure water, a scientific issue under debate
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2017 (English)In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 122, p. 53-60Article in journal (Refereed) Published
Abstract [en]

The corrosion properties of copper in ultrapure water have been studied experimentally by submerging copper samples (99.9999%) in pure water for up to 29 months. The surface was first electropolished at ambient temperature, then exposed to hydrogen gas treatment at 300-400 degrees C, thereby reducing the bulk hydrogen content to 0.03 ppm. These copper samples, the water and the glassware were all then subjected to precise chemical analysis. Great care was taken to avoid contamination. After exposure, only similar to 6 mu g/L copper had accumulated in the water phase. Electron spectroscopy could not detect Cu2O or any other oxidation products containing copper.

Place, publisher, year, edition, pages
PERGAMON-ELSEVIER SCIENCE LTD, 2017
Keywords
Copper, XPS, AES, Oxidation
National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-330714 (URN)10.1016/j.corsci.2017.03.014 (DOI)000404490600006 ()
Available from: 2017-10-09 Created: 2017-10-09 Last updated: 2017-12-28Bibliographically approved
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Identifiers
ORCID iD: ORCID iD iconorcid.org/0000-0002-7018-9617

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