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An X-ray Spectroscopic Study of Perovskites Oxides and Halides for Emerging Devices
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Molecular and Condensed Matter Physics.ORCID iD: 0000-0003-0351-3138
2018 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis investigates the electronic structures on several perovskite oxide and halide materials with a focus on light harvesting applications. The systematic study of the electronic properties of the transition metal oxides and post-transition metal halides is a key point if one is to understand their properties. The element and site selective nature of several x-ray based spectroscopic techniques are given special emphasis in order to obtain a complete picture of the electronic properties of the compounds in question. Much of the experimental studies are accompanied by ab initio calculations that corroborate with our experimental results.

In the oxide portion of this work, a new class of metallic oxides based on doping of an antiferromagnetic LaFeO3 was synthesized and systematically studied with x-ray absorption, x-ray emission, and photoemission spectroscopies. The compound’s electronic structure is complex, having itinerant as well as localized components that give rise to a unique physical state where antiferromagnetism, metallicity and charge-disproportionation coexist. Our resonant photoemission results establish that the Fe states in both magnetically ordered oxides show insulting properties, while the Mo states provide an itinerant band crossing the Fermi level. An excitation energy-dependent RIXS investigation on LaFe1-xMoxO3 and the double perovskite Sr2FeMoO6 revealed a double peak structure located in proximity to the elastic peak that is identified to purely d-d excitations, attributed to the strongly correlated nature of these transition metal compounds.

The growth of high-quality thin film ferroelectric based on BaTiO3 grown epitaxially by means of pulsed laser deposition were investigated. We systematically reduce the band gap of the ferroelectric thin film while retaining its polarization at ambient conditions in spite of the aliovalent doping. The electronic structure is studied by several x-ray techniques that show how the ferroelectricity persists as well as the effective reduction of the band gap through hybridized states.

In the post-transition metal halides, the valence and conduction bands were mapped using x-ray absorption, emission, and photoemission spectroscopies. The spectroscopic results identify the constituent states that form the valence band as well as the band energy positions, which is an imperative parameter in optoelectronic devices. In addition, x-ray based spectroscopy was used to demonstrate the stereochemical activity of lone-pair states (5s2 and 6s2) for several different halide compounds and their influence on the chemical, structural, and electronic properties of the material. Nanostructured halide perovskites are also explored. The position of iodine p states and valence band states in reduced dimensional lead-based compounds were examined, as their states are found to be confined in one crystallographic direction in contrast to their three-dimensional counterpart. This information highlights the interesting material properties and their use in current third generation solar cell research.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2018. , p. 84
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1740
Keywords [en]
perovskite oxides, halide perovskites, x-ray spectroscopy, electronic structure
National Category
Condensed Matter Physics
Research subject
Physics with spec. in Atomic, Molecular and Condensed Matter Physics
Identifiers
URN: urn:nbn:se:uu:diva-364407ISBN: 978-91-513-0493-9 (print)OAI: oai:DiVA.org:uu-364407DiVA, id: diva2:1258875
Public defence
2018-12-14, Häggsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 13:15 (English)
Opponent
Supervisors
Available from: 2018-11-21 Created: 2018-10-26 Last updated: 2018-11-30
List of papers
1. Electronic structure of the charge disproportionate and metallicity in LaFe1-xMoxO3 studied by resonant x-ray spectroscopies
Open this publication in new window or tab >>Electronic structure of the charge disproportionate and metallicity in LaFe1-xMoxO3 studied by resonant x-ray spectroscopies
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

A metal-insulator transition and its intriguing properties were recently reported based on doping of the antiferromagnetic insulator LaFeO3. Through doping at the B site by Mo to the insulating perovskite LaFeO3 exhibits a coexistence of an antiferromagnetic ordering with room-temperature metallicity at higher doping levels, an unusual ground state for an oxide perovskite. Replacing Fe by Mo in the Fe-O6 octahedra enhances the separation of the two 2 Fe-O bonds relative to the orthorhombic LaFeO3, largely retaining the centrosymmetric character of the Fe sites, as confirmed through extended x-ray absorption fine structure. Mo ions appear to be homogeneously doped, with average valency of both metal sites monotonically decreasing with increasing Mo concentration. Resonant photoemission was recorded for both Fe and Mo to obtain element specific spectral information on the projected 3d and 4d partial density of states. The data shows gradual increase of spectral weight at the Fermi level that is attributed to Mo d states, while the Fe d states primarily reside at higher binding energy in the valence band, with significant hybridization with O 2p states. The RIXS spectra show strong electron correlation effects from d-d inelastic features and broad charge-transfer excitations for x = 0.2 where the compound becomes metallic. This is in contrast to the insulating parent LaFeO3 compound and insulating samples with lower Mo content. The coexistence of both bound and continuum excitations observed in the RIXS spectra provides strong evidence for charge disproportionation with features that are linked to the disproportionate Fe sites.

National Category
Condensed Matter Physics
Research subject
Physics with spec. in Atomic, Molecular and Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-364367 (URN)
Funder
Knut and Alice Wallenberg Foundation, 2012.0031Swedish Energy Agency, P45349-1Swedish Research Council, 2014-6019Carl Tryggers foundation , CTS-17:376
Available from: 2018-10-25 Created: 2018-10-25 Last updated: 2018-10-26
2. Valence electronic structure of the double perovskite Sr2FeMoO6 through resonant x-ray spectroscopies
Open this publication in new window or tab >>Valence electronic structure of the double perovskite Sr2FeMoO6 through resonant x-ray spectroscopies
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

Resonant x-ray spectroscopies were used to investigate the double perovskite Sr2FeMoO6 (SFMO) in order to identify the compounds valence electronic structure known for its half-metallicity and ferrimagnetism above room temperature. A comprehensive resonant photoelectron spectroscopy (RPES) and resonant inelastic x-ray scattering (RIXS) study was carried out to acquire a more detailed understanding and interpretation of the valence band electronic structure and hybridization between Fe and Mo d bands. The RPES spectrum clearly show enhancement of Mo d states at the Fermi level that are partly responsible for the metallic behavior. The RPES data at the Fe L3 edge shows strong hybridization with O 2p states as well hybridization with Mo d states. At the same time, characteristic d-d excitations are observed in the RIXS spectra at the Fe L edge indicative of Fe d states of more localized character. Although there are many valid definitions to the valency of the Fe and Mo ions and magnetic moments, the total electronic structure represented through element-resolved x-ray spectroscopies studies distinctly identifies the electronic states that results in its established correlated behavior and half-metallicity.

National Category
Condensed Matter Physics
Research subject
Physics with spec. in Atomic, Molecular and Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-364368 (URN)
Funder
Carl Tryggers foundation , CTS-17:376Swedish Energy Agency, P43549-1Swedish Research Council, 2016-4524Knut and Alice Wallenberg Foundation, 2012.0031Swedish Foundation for Strategic Research , 15-0130
Available from: 2018-10-25 Created: 2018-10-25 Last updated: 2018-10-26
3. The origin of low bandgap and ferroelectricity of a co-doped BaTiO3
Open this publication in new window or tab >>The origin of low bandgap and ferroelectricity of a co-doped BaTiO3
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2018 (English)In: Europhysics letters, ISSN 0295-5075, E-ISSN 1286-4854, Vol. 124, no 2, article id 27005Article in journal (Refereed) Published
Abstract [en]

We recently demonstrated the lowest bandgap bulk ferroelectric material, BaTi1-x(Mn1/2Nb1/2)xO3, a promising candidate material for visible light absorption in opto- electronic devices. Using a combination of x-ray spectroscopies and density functional theory (DFT) calculations, we here elucidate this compound’s electronic structure and the modifications induced by Mn doping. In particular, we are able to rationalize how this compound retains its ferroelectricity even through a significant reduction of the optical gap upon Mn doping. The local electronic structure and atomic coordination are investigated using x-ray absorption at the Ti K, Mn K, and O K edges, which suggests only small distortions to the parent tetragonal ferroelectric system, BaTiO3, thereby providing a clue to the substantial retention of ferroelectricity in spite of doping. Features at the Ti K edge, which are sensitive to local symmetry and an indication of Ti off-centering within the Ti-O6 octahedra, show modest changes with doping and strongly corroborates with our measured polarization values. Resonant photoelectron spectroscopy results suggest the origin of the reduction of the bandgap in terms of newly created Mn d bands that hybridize with O 2p states. X-ray absorption spectra at the O K-edge provide evidence for new states below the conduction band of the parent compound, illustrating additional contributions facilitating bandgap reduction.

National Category
Condensed Matter Physics
Research subject
Physics with spec. in Atomic, Molecular and Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-364369 (URN)10.1209/0295-5075/124/27005 (DOI)000450630500002 ()
Funder
Swedish Foundation for Strategic Research , 15-0130Knut and Alice Wallenberg Foundation, 2012.0031Swedish Energy Agency, P43549-1Swedish Energy Agency, P43294-1Swedish Research Council, 2014-7019Swedish Research Council, 2016-4524
Note

Corection in: EPL, Volume: 124, Issue: 6, Article Number: 69901, DOI: 10.1209/0295-5075/124/69901

Available from: 2018-10-25 Created: 2018-10-25 Last updated: 2019-02-04Bibliographically approved
4. Ferroelectric properties of doped BaTiO3 thin film by pulsed laser deposition
Open this publication in new window or tab >>Ferroelectric properties of doped BaTiO3 thin film by pulsed laser deposition
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

BaTiO3 thin films co-doped at the Ti site with Mn and Nb were grown on 0.5% Nb-doped (001) oriented SrTiO3 substrates by pulsed laser deposition. The films show single-phase tetragonal structure, growing epitaxially with a smooth interface to the substrate. Using piezoforce microscopy, we find that both doped and undoped films exhibit good ferroelectric response. The piezoelectric domain switching in the films was confirmed by measuring local hysteresis of the polarization at several different areas across the thin films, demonstrating a switchable ferroelectric state for these films. The doping of the BaTiO3 also reduces the bandgap of the material from 3.18 eV for BaTiO3 to nearly 2.7 eV for the 7.5% doped sample, potentially making the films effective light-harvesters in the visible spectrum. The results demonstrate co-doping as an effective strategy for bandgap engineering and a guide for the realization of visible-light applications of related thin film systems.

National Category
Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-364370 (URN)
Funder
Swedish Research Council, 2014-6019Swedish Research Council, 2016-4524Swedish Energy Agency, P43549-1Knut and Alice Wallenberg Foundation, 2012.0031Swedish Foundation for Strategic Research , 15-0130
Available from: 2018-10-25 Created: 2018-10-25 Last updated: 2018-10-26
5. Impact of synthetic routes on the structural and physical properties of butyl-1,4-diammonium lead iodide semiconductors
Open this publication in new window or tab >>Impact of synthetic routes on the structural and physical properties of butyl-1,4-diammonium lead iodide semiconductors
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2017 (English)In: Journal of Materials Chemistry A, ISSN 2050-7488, Vol. 5, no 23, p. 11730-11738Article in journal (Refereed) Published
Abstract [en]

We report the significant role of synthetic routes and the importance of solvents in the synthesis of organic-inorganic lead iodide materials. Through one route, the intercalation of dimethylformamide in the crystal structure was observed leading to a one-dimensional (1D) [NH3(CH2)(4)NH3]Pb2I6 structure of the product. This product was compared with the two-dimensional (2D) [NH3(CH2)(4)NH3]PbI4 recovered from aqueous solvent based synthesis with the same precursors. UV-visible absorption spectroscopy showed a red-shift of 0.1 eV for the band gap of the 1D network in relation to the 2D system. This shift primarily originates from a shift in the valence band edge as determined from photoelectron-and X-ray spectroscopy results. These findings also suggest the iodide 5p orbital as the principal component in the density of states in the valence band edge. Single crystal data show a change in the local coordination around iodide, while in both materials, lead atoms are surrounded by iodide atoms in octahedral units. The conductivity of the one-dimensional material ([NH3(CH2)(4)NH3]Pb2I6) was 50% of the two-d(i)mensional material ([NH3(CH2)(4)NH3]PbI4). The fabricated solar cells reflect these changes in the chemical and electronic structure of both materials, although the total light conversion efficiencies of solar cells based on both products were similar.

Place, publisher, year, edition, pages
ROYAL SOC CHEMISTRY, 2017
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-329653 (URN)10.1039/c6ta10123b (DOI)000403228200030 ()
Funder
StandUpSwedish Energy AgencySwedish Research CouncilKnut and Alice Wallenberg Foundation
Available from: 2017-09-20 Created: 2017-09-20 Last updated: 2018-10-26Bibliographically approved
6. Electronic Structure of Two-Dimensional Lead(II) Iodide Perovskites: An Experimental and Theoretical Study
Open this publication in new window or tab >>Electronic Structure of Two-Dimensional Lead(II) Iodide Perovskites: An Experimental and Theoretical Study
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2018 (English)In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 30, no 15, p. 4959-4967Article in journal (Refereed) Published
Abstract [en]

Layered two-dimensional (2D) hybrid organic-inorganic perovskites (HOP) are promising materials for light-harvesting applications because of their chemical stability, wide flexibility in composition and dimensionality, and increases in photovoltaic power conversion efficiencies. Three 2D lead iodide perovskites were studied through various X-ray spectroscopic techniques to derive detailed electronic structures and band energetics profiles at a titania interface. Core-level and valence band photoelectron spectra of HOP were analyzed to resolve the electronic structure changes due to the reduced dimensionality of inorganic layers. The results show orbital narrowing when comparing the HOP, the layered precursor PbI2, and the conventional 3D (CH3NH3)PbI3 such that different localizations of band edge states and narrow band states are unambiguously due to the decrease in dimensionality of the layered HOPs. Support from density functional theory calculations provide further details on the interaction and band gap variations of the electronic structure. We observed an interlayer distance dependent dispersion in the near band edge electronic states. The results show how tuning the interlayer distance between the inorganic layers affects the electronic properties and provides important design principles for control of the interlayer charge transport properties, such as the change in effective charge masses as a function of the organic cation length. The results of these findings can be used to tune layered materials for optimal functionality and new applications.

National Category
Condensed Matter Physics Engineering and Technology
Identifiers
urn:nbn:se:uu:diva-361922 (URN)10.1021/acs.chemmater.8b00909 (DOI)000442186500014 ()
Funder
StandUpSwedish Energy AgencySwedish Research CouncilKnut and Alice Wallenberg Foundation
Note

De två första författarna delar förstaförfattarskapet.

Available from: 2018-09-27 Created: 2018-09-27 Last updated: 2018-11-02Bibliographically approved
7. The electronic structure and band interface of cesium bismuth iodide on a titania heterostructure using hard X-ray spectroscopy
Open this publication in new window or tab >>The electronic structure and band interface of cesium bismuth iodide on a titania heterostructure using hard X-ray spectroscopy
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2018 (English)In: Journal of Materials Chemistry A, ISSN 2050-7488, Vol. 6, no 20, p. 9498-9505Article in journal (Refereed) Published
Abstract [en]

Bismuth halide compounds as a non-toxic alternative are increasingly investigated because of their potential in optoelectronic devices and their rich structural chemistry. Hard X-ray spectroscopy was applied to the ternary bismuth halide Cs3Bi2I9 and its related precursors BiI3 and CsI to understand its electronic structure at an atomic level. We specifically investigated the core levels and valence band using X-ray photoemission spectroscopy (PES), high-resolution X-ray absorption (HERFD-XAS), and resonant inelastic X-ray scattering (RIXS) to get insight into the chemistry and the band edge properties of the two bismuth compounds. Using these element specific X-ray techniques, our experimental electronic structures show that the primary differences between the two bismuth samples are the position of the iodine states in the valence and conduction bands and the degree of hybridization with bismuth lone pair (6s(2)) states. The crystal structure of the two layered quasi-perovskite compounds plays a minor role in modifying the overall electronic structure, with variations in bismuth lone pair states and iodine band edge states. Density Functional Theory (DFT) calculations are used to compare with experimental data. The results demonstrate the effectiveness of hard X-ray spectroscopies to identify element specific bulk electronic structures and their use in optoelectronic devices.

National Category
Materials Chemistry Physical Chemistry
Identifiers
urn:nbn:se:uu:diva-357561 (URN)10.1039/c8ta00947c (DOI)000433427300020 ()
Funder
Swedish Research Council, 2014-6019Swedish Research Council, 2016-4524Swedish Energy Agency, P43549-1Swedish Foundation for Strategic Research , 15-0130Wallenberg Foundations, 2012.0031StandUp
Available from: 2018-08-20 Created: 2018-08-20 Last updated: 2019-02-19Bibliographically approved
8. An effective approach of vapour assisted morphological tailoring for reducing metal defect sites in lead-free, (CH3NH3)(3)Bi2I9 bismuth-based perovskite solar cells for improved performance and long-term stability
Open this publication in new window or tab >>An effective approach of vapour assisted morphological tailoring for reducing metal defect sites in lead-free, (CH3NH3)(3)Bi2I9 bismuth-based perovskite solar cells for improved performance and long-term stability
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2018 (English)In: Nano Energy, ISSN 2211-2855, E-ISSN 2211-3282, Vol. 49, p. 614-624Article in journal (Refereed) Published
Abstract [en]

We present a controlled, stepwise formation of methylammonium bismuth iodide (CH3NH3)(3)Bi2I9 perovskite films prepared via the vapour assisted solution process (VASP) by exposing BiI3 films to CH3NH3I (MAI) vapours for different reaction times, (CH3NH3)(3)Bi2I9 semiconductor films with tunable optoelectronic properties are obtained. Solar cells prepared on mesoporous TiO2 substrates yielded hysteresis-free efficiencies upto 3.17% with good reproducibility. The good performance is attributed mainly to the homogeneous surface coverage, improved stoichiometry, reduced metallic content in the bulk, and desired optoelectronic properties of the absorbing material. In addition, solar cells prepared using pure BiI3 films without MAI exposure achieved a power conversion efficiency of 0.34%. The non-encapsulated (CH3NH3)(3)Bi2I9 devices were found to be stable for as long as 60 days with only 0.1% drop in efficiency. This controlled formation of (CH3NH3)(3)Bi2I9 perovskite films highlights the benefit of the VASP technique to optimize material stoichiometry, morphology, solar cell performance, and long-term durability.

Place, publisher, year, edition, pages
ELSEVIER SCIENCE BV, 2018
Keywords
Vapour assisted solution process (VASP), Lead free perovskite, (CH3NH3)(3)Bi2I9, Morphological tailoring, High resolution X-ray photoelectron (HAXPES) spectroscopy
National Category
Materials Chemistry Condensed Matter Physics Engineering and Technology
Identifiers
urn:nbn:se:uu:diva-358277 (URN)10.1016/j.nanoen.2018.05.003 (DOI)000434829500071 ()
Funder
Swedish Research CouncilEU, Horizon 2020, 663830
Available from: 2018-08-27 Created: 2018-08-27 Last updated: 2018-10-26Bibliographically approved
9. Inorganic CsPbI3 Perovskite Coating on PbS Quantum Dot for Highly Efficient and Stable Infrared Light Converting Solar Cells
Open this publication in new window or tab >>Inorganic CsPbI3 Perovskite Coating on PbS Quantum Dot for Highly Efficient and Stable Infrared Light Converting Solar Cells
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2018 (English)In: Advanced Energy Materials, ISSN 1614-6832, Vol. 8, no 6, article id 1702049Article in journal (Refereed) Published
Abstract [en]

Solution-processed colloidal quantum dot (CQD) solar cells harvesting the infrared part of the solar spectrum are especially interesting for future use in semitransparent windows or multilayer solar cells. To improve the device power conversion efficiency (PCE) and stability of the solar cells, surface passivation of the quantum dots is vital in the research of CQD solar cells. Herein, inorganic CsPbI3 perovskite (CsPbI3-P) coating on PbS CQDs with a low-temperature, solution-processed approach is reported. The PbS CQD solar cell with CsPbI3-P coating gives a high PCE of 10.5% and exhibits remarkable stability both under long-term constant illumination and storage under ambient conditions. Detailed characterization and analysis reveal improved passivation of the PbS CQDs with the CsPbI3-P coating, and the results suggest that the lattice coherence between CsPbI3-P and PbS results in epitaxial induced growth of the CsPbI3-P coating. The improved passivation significantly diminishes the sub-bandgap trap-state assisted recombination, leading to improved charge collection and therefore higher photovoltaic performance. This work therefore provides important insight to improve the CQD passivation by coating with an inorganic perovskite ligand for photovoltaics or other optoelectronic applications.

Place, publisher, year, edition, pages
WILEY-V C H VERLAG GMBH, 2018
Keywords
charge recombination, inorganic perovskite, quantum dots, solar cells, surface passivation
National Category
Physical Chemistry Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-348982 (URN)10.1002/aenm.201702049 (DOI)000426152400017 ()
Funder
Swedish Energy AgencySwedish Research CouncilSwedish Research Council Formas
Available from: 2018-04-26 Created: 2018-04-26 Last updated: 2019-09-26
10. Doping induced site-selective Mott insulating phase in LaFeO3
Open this publication in new window or tab >>Doping induced site-selective Mott insulating phase in LaFeO3
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(English)Manuscript (preprint) (Other academic)
Abstract [en]

Tailoring transport properties of strongly correlated electron systems in a controlled fashion counts among the dreams of materials scientists. In copper oxides, vary- ing the carrier concentration is a tool to obtain high- temperature superconducting phases. In manganites, dop- ing results in exotic physics such as insulator-metal tran- sitions (IMT), colossal magnetoresistance (CMR), orbital- or charge-ordered (CO) or charge-disproportionate (CD) states. In most oxides, antiferromagnetic order and CD phase is asssociated with insulating behavior. Here we re- port the realization of a unique physical state that can be induced by Mo doping in LaFeO3: the resulting metallic state is a site-selective Mott insulator where itinerant elec- trons evolving on low-energy Mo states coexist with local- ized carriers on the Fe sites. In addition, a local breathing- type lattice distortion induces charge disproportionation on the latter, without destroying the antiferromagnetic order. A state, combining antiferromangetism, metallic- ity and CD phenomena is rather rare in oxides and have utmost significance for future antiferromagnetic memory devices.

National Category
Condensed Matter Physics
Research subject
Physics with spec. in Atomic, Molecular and Condensed Matter Physics
Identifiers
urn:nbn:se:uu:diva-364365 (URN)
Funder
Swedish Research Council, 2014-6019Swedish Energy Agency, P43549-1Knut and Alice Wallenberg Foundation, 2012.0031
Available from: 2018-10-25 Created: 2018-10-25 Last updated: 2018-11-01

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