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Bakhiia, T., Gurzęda, B., Li, G., Boulanger, N., Maslakov, K., Krot, A., . . . Talyzin, A. V. (2025). Extraordinary U(vi) sorption capacity of high surface area super-oxidized carbons. Materials Advances
Open this publication in new window or tab >>Extraordinary U(vi) sorption capacity of high surface area super-oxidized carbons
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2025 (English)In: Materials Advances, E-ISSN 2633-5409Article in journal (Refereed) Epub ahead of print
Abstract [en]

Porous carbons based on activated reduced graphene oxide (rGO) have been demonstrated as excellent sorbents for U(vi), with their sorption capacity correlating with the degree of their oxidation. Herein, we demonstrate an extraordinarily high U(vi) sorption of ∼7050 μmol g−1 for super-oxidized porous carbon (SOPC) with a specific surface area (SSA) of ∼970 m2 g−1 and an extremely high degree of oxidation (C/O = 2.1), similar to graphene oxide. The SOPC materials were prepared using an oxidation treatment applied to activated carbon produced from spruce cones. The extremely high SSA of the precursor activated carbon (∼3400 m2 g−1) as well as its microporous structure and mild oxidation treatment allowed for the preservation of a significant part of the surface area, providing materials with rather narrow pore size distribution (∼7.5 Å). The SOPC prepared from spruce cone biochar is similar to defective graphene oxide but with a significantly higher surface area, resulting in superior U(vi) sorption. Analysis of EXAFS and XPS data shows that U(vi) likely binds to carboxylic groups on the opposite sides of the micropores. The small size of the micropores and irregular pore wall structure are the main factors affecting pore sorption. The spruce-cone biochar has a strong advantage compared with earlier used rGO as a precursor for the preparation of SOPC.

Place, publisher, year, edition, pages
Royal Society of Chemistry, 2025
National Category
Materials Chemistry
Identifiers
urn:nbn:se:umu:diva-239121 (URN)10.1039/d5ma00277j (DOI)001484331900001 ()2-s2.0-105004809645 (Scopus ID)
Funder
Carl Tryggers foundation The Kempe Foundations
Available from: 2025-05-27 Created: 2025-05-27 Last updated: 2025-05-27
Iakunkov, A., Boulanger, N., Gurzęda, B., Li, G., Hennig, C., Svitlyk, V., . . . Talyzin, A. V. (2025). In situ x-ray diffraction study of MXene synthesis by the reaction of Ti3AlC2 with molten zinc and tin chlorides. Chemistry of Materials, 37(3), 1132-1142
Open this publication in new window or tab >>In situ x-ray diffraction study of MXene synthesis by the reaction of Ti3AlC2 with molten zinc and tin chlorides
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2025 (English)In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 37, no 3, p. 1132-1142Article in journal (Refereed) Published
Abstract [en]

Using molten salts for etching aluminum (Al) away from the MAX phase for MXene synthesis is an attractive alternative method that allows one to avoid the use of toxic hydrofluoric acid (HF) solutions. However, the mechanism of the MAX phase reaction with molten salts remains to date unclear due to the lack of in situ data. Here, we present a detailed in situ time-resolved synchrotron radiation X-ray diffraction study of the MAX phase annealing in molten ZnCl2 and SnCl2. The reaction of salts with the MAX phase is found to occur in two stages. The initial period of annealing results in the delamination of two-dimensional (2D) Ti3C2 layers, vigorous evolution of AlCl3 bubbles, and dissolution of Zn in a ZnCl2 melt. The chlorine-terminated Ti3C2 sheets formed in the delaminated state are restacked into a relatively well-ordered MXene structure (P63/mmc, a = 3.071 Å and c = 18.577 Å) during the prolonged annealing in molten salts. Surprisingly, the data recorded directly in molten salts at temperatures up to 873 K demonstrate that Ti3C2Clx MXene shows no swelling in both liquid ZnCl2 and SnCl2. The structure of MXene studied directly in the molten salts is found to be the same as in ex situ experiments performed after cooling and water washing under ambient conditions. The absence of the “pristine” melt-swollen phase indicates a rather different mechanism of MXene formation compared to HF-based solution methods. Formation of MXene by gradually removing Al from the MAX phase starting at the edges of flakes and propagating into the deeper parts of interlayers is not possible, since the molten salt is not capable of penetrating between Cl-terminated Ti3C2 layers.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2025
National Category
Materials Chemistry Inorganic Chemistry
Identifiers
urn:nbn:se:umu:diva-234887 (URN)10.1021/acs.chemmater.4c02989 (DOI)001401451000001 ()2-s2.0-85215866707 (Scopus ID)
Funder
Swedish Energy Agency, 50620-1Swedish Energy Agency, 48489-1The Kempe FoundationsSwedish Research Council, 2018-07152Vinnova, 2018-04969Swedish Research Council Formas, 2019-02496
Available from: 2025-02-11 Created: 2025-02-11 Last updated: 2025-02-11Bibliographically approved
Li, G., Gurzęda, B., Iakunkov, A., Nordenström, A., Boulanger, N., Hennig, C., . . . Talyzin, A. V. (2025). Temperature dependent swelling transitions of hummers graphite oxide in liquid 1-Alcohols. Advanced Materials Interfaces, 12(6), Article ID 202400651.
Open this publication in new window or tab >>Temperature dependent swelling transitions of hummers graphite oxide in liquid 1-Alcohols
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2025 (English)In: Advanced Materials Interfaces, ISSN 2196-7350, Vol. 12, no 6, article id 202400651Article in journal (Refereed) Published
Abstract [en]

Graphite oxides (GO) swell in liquid alcohols with significant expansion of c-lattice. However, temperature-dependent swelling of Hummers GO (HGO) has so far been reported only for methanol and ethanol. Here, HGO swelling in liquid 1-alchohols (C1 to C22 according to the number of carbons) is studied as a function of temperature using in situ synchrotron radiation XRD. Swelling transitions never previously observed for HGO in any kind of polar solvents are found, enthalpy of these transition and compositions of HGO-Cx solid solvates near the point of solvent melting reported. Swelling transitions from low temperature to high-temperature phase are found for HGO in C10–C22 alcohols, similarly to earlier reported transitions in Brodie graphite oxide (BGO). The transitions correspond to a strong change of inter-layer distance correlating with the alcohol molecules length and change in molecules orientation from perpendicular to parallel to GO planes (Type II transitions). However, Type I swelling transitions (related to insertion/removal of one layer of alcohol molecules) reported earlier for BGO are not found in HGO. Continuous changes of the d(001) spacing are revealed for HGO immersed in all smaller alcohols in the range C1 (methanol) to C9 (nonanol).

Place, publisher, year, edition, pages
John Wiley & Sons, 2025
Keywords
alcohols, graphene, graphene oxide, swelling, X-ray diffraction
National Category
Condensed Matter Physics
Identifiers
urn:nbn:se:umu:diva-230123 (URN)10.1002/admi.202400651 (DOI)001321069800001 ()2-s2.0-85204677425 (Scopus ID)
Funder
EU, Horizon 2020, 881603Swedish Energy Agency, 50620–1Swedish Research Council, 2018–07152Vinnova, 2018–04969Swedish Research Council Formas, 2019–02496
Available from: 2024-10-14 Created: 2024-10-14 Last updated: 2025-04-14Bibliographically approved
Boulanger, N., Jia, X., Yaghini, N., Sharifi, T., Bengtsson, E., Trey, S. & Wågberg, T. (2024). Aramid based slot liners for low voltage electric motor applications. In: 2024 IEEE Electrical Insulation Conference (EIC): . Paper presented at 2024 IEEE Electrical Insulation Conference, EIC 2024, Minneapolis, USA, June 2-5, 2024 (pp. 17-21). IEEE
Open this publication in new window or tab >>Aramid based slot liners for low voltage electric motor applications
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2024 (English)In: 2024 IEEE Electrical Insulation Conference (EIC), IEEE, 2024, p. 17-21Conference paper, Published paper (Refereed)
Abstract [en]

The insulation in the stator of a low voltage electric motor has a double purpose: ensuring the electric insulation around the stator wiring as well as permitting a good evacuation of the generated heat. Improving the heat transfer properties of the slot liner within the stator while maintaining its electrical insulation properties allows for more efficient electric motors. This paper presents different types of composites based on an aramid matrix with boron nitride, zinc oxide and aluminum oxide fillers. The effect of the different filler materials on the thermal conductivity and the electric insulation properties of the slot liner are presented. Perspectives on the needs for a life cycle assessment of the slot liner constituents are evoked.

Place, publisher, year, edition, pages
IEEE, 2024
Series
IEEE Electrical Insulation Conference, ISSN 2993-3676, E-ISSN 2993-3684
Keywords
electric motor, slot liner, thermal conductivity
National Category
Other Electrical Engineering, Electronic Engineering, Information Engineering
Identifiers
urn:nbn:se:umu:diva-228083 (URN)10.1109/EIC58847.2024.10579397 (DOI)001270314100074 ()2-s2.0-85199112323 (Scopus ID)979-8-3503-6043-1 (ISBN)979-8-3503-6044-8 (ISBN)
Conference
2024 IEEE Electrical Insulation Conference, EIC 2024, Minneapolis, USA, June 2-5, 2024
Funder
Swedish Energy Agency, 2021-037097
Available from: 2024-08-01 Created: 2024-08-01 Last updated: 2025-04-24Bibliographically approved
Iakunkov, A., Nordenström, A., Boulanger, N., Li, G., Hennig, C., Jørgensen, M. R., . . . Talyzin, A. V. (2024). Effect of chain length on swelling transitions of Brodie graphite oxide in liquid 1-alcohols. Advanced Materials Interfaces, 11(1), Article ID 2300554.
Open this publication in new window or tab >>Effect of chain length on swelling transitions of Brodie graphite oxide in liquid 1-alcohols
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2024 (English)In: Advanced Materials Interfaces, ISSN 2196-7350, Vol. 11, no 1, article id 2300554Article in journal (Refereed) Published
Abstract [en]

Swelling is the most fundamental property of graphite oxides (GO). Here, a structural study of Brodie graphite oxide (BGO) swelling in a set of long chain 1-alcohols (named C11 to C22 according to the number of carbons) performed using synchrotron radiation X-ray diffraction at elevated temperatures is reported. Even the longest of tested alcohols (C22) is found to intercalate BGO with enormous expansion of the interlayer distance from ≈6Å up to ≈63Å, the highest expansion of GO lattice ever reported. Swelling transitions from low temperature α-phase to high temperature β-phase are found for BGO in all alcohols in the C11–C22 set. The transitions correspond to decrease of inter-layer distance correlating with the length of alcohol molecules, and change in their orientation from perpendicular to GO planes to layered parallel to GO (Type II transitions). These transitions are very different compared to BGO swelling transitions (Type I) found in smaller alcohols and related to insertion/de-insertion of additional layer of alcohol parallel to GO. Analysis of general trends in the whole set of 1-alcohols (C1 to C22) shows that the 1-alcohol chain length defines the type of swelling transition with Type I found for alcohols with C<10 and Type II for C>10. 

Place, publisher, year, edition, pages
Wiley-VCH Verlagsgesellschaft, 2024
Keywords
alcohols, graphene, graphene oxide, swelling, X-ray diffraction
National Category
Condensed Matter Physics Physical Chemistry
Identifiers
urn:nbn:se:umu:diva-214114 (URN)10.1002/admi.202300554 (DOI)001085318300001 ()2-s2.0-85174293807 (Scopus ID)
Funder
EU, Horizon 2020, 881603Swedish Energy Agency, 50620‐1Swedish Research Council, 2018‐07152Vinnova, 2018‐04969Swedish Research Council Formas, 2019‐02496
Note

Originally included in thesis in manuscript form. 

This article also appears in: Advanced Materials Interfaces Editors' Choice.

Available from: 2023-09-05 Created: 2023-09-05 Last updated: 2024-08-19Bibliographically approved
Gurzęda, B., Boulanger, N., Jørgensen, M. R. .., Kantor, I. & Talyzin, A. V. (2024). Graphite oxide by “chlorate route” oxidation without HNO3: Does acid matter?. Carbon, 221, Article ID 118899.
Open this publication in new window or tab >>Graphite oxide by “chlorate route” oxidation without HNO3: Does acid matter?
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2024 (English)In: Carbon, ISSN 0008-6223, E-ISSN 1873-3891, Vol. 221, article id 118899Article in journal (Refereed) Published
Abstract [en]

Very strong difference in many properties is well documented for graphite oxides (GtO) synthesized by Brodie (BGO) and Hummers (HGO) methods. The difference is typically assigned to the type of oxidant (chlorates or KMnO4, respectively). However, not only oxidants but also acids used in these methods are different. It is still unclear which of the different properties of GtO are dependent on the oxidant or acid used in the synthesis. Here we synthesized a new type of graphite oxide using an oxidation agent typical for the Brodie method (KClO3) in combination with acids so far used only in modified Hummers' method (H2SO4+H3PO4). The GtO synthesized by this method (MGO) demonstrates some properties similar to BGO (higher temperature of exfoliation and less defected structure) but also similarity to some other properties of HGO (absence of sharp swelling transitions). Comparing MGO, BGO, and HGO allows us to distinguish the effects of acids and oxidants on the properties of graphite oxides. The new procedure proposed in this study allows preparation of GtO nearly free from hole/vacancy defects (similarly to BGO) but avoids dangerous HNO3. MGO is suggested as a favorable precursor for the preparation of graphene films by thermal or chemical reduction methods.

Keywords
Chemical oxidation, Graphene oxide, Graphite, Graphite oxide, Swelling
National Category
Condensed Matter Physics Materials Chemistry
Identifiers
urn:nbn:se:umu:diva-221389 (URN)10.1016/j.carbon.2024.118899 (DOI)001184711900001 ()2-s2.0-85184999821 (Scopus ID)
Funder
Swedish Energy Agency, 50620-1The Kempe Foundations
Available from: 2024-02-27 Created: 2024-02-27 Last updated: 2025-04-24Bibliographically approved
Boulanger, N., Talyzin, A. V., Xiong, S., Hultberg, M. & Grimm, A. (2024). High surface area activated carbon prepared from wood-based spent mushroom substrate for supercapacitors and water treatment. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 680, Article ID 132684.
Open this publication in new window or tab >>High surface area activated carbon prepared from wood-based spent mushroom substrate for supercapacitors and water treatment
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2024 (English)In: Colloids and Surfaces A: Physicochemical and Engineering Aspects, ISSN 0927-7757, E-ISSN 1873-4359, Vol. 680, article id 132684Article in journal (Refereed) Published
Abstract [en]

Edible white-rot fungi are commonly cultivated on wood-based substrates and selectively degrade lignin to a larger extent during their growth. Spent mushroom substrate (SMS) is produced in huge amounts by the mushroom industry and today there is a lack of proven methods to valorize this kind of biomass waste, which in most cases is landfilled or used as fuel. This study demonstrates that birch wood-based SMS from the cultivation of oyster mushrooms can be converted into high-quality activated carbon (AC) with an extremely high surface area of about 3000 m2/g. These activated carbons showed good performance when used in electrodes for supercapacitors, with energy storage parameters nearly identical to AC produced from high-quality virgin birch wood. Moreover, AC produced from SMS showed high potential as an adsorbent for cleaning reactive orange-16 azo dye from aqueous solutions as well as contaminants from synthetic effluents and from real sewage water. The kinetics of adsorption were well represented by the Avrami fractional order model and isotherms of adsorption by the Liu model. The theoretical maximum reactive orange-16 adsorption capacities were approximately 519 mg/g (SMS-based carbon) and 553 mg/g (virgin birch-based carbon). The removal of contaminants from synthetic effluents made of different dyes and inorganic compounds was around 95% and 83% depending on the effluent composition. The removal of contaminants from raw sewage water was around 84%, and from treated sewage water was around 68%. Overall, the results showed that activated carbon prepared from waste generated during cultivation of white-rot fungi is as good as activated carbon prepared from high-quality virgin wood.

Place, publisher, year, edition, pages
Elsevier, 2024
Keywords
Activated carbon, Adsorbents, Spent mushroom substrate, Supercapacitors, Water treatment
National Category
Environmental Sciences
Identifiers
urn:nbn:se:umu:diva-216654 (URN)10.1016/j.colsurfa.2023.132684 (DOI)001110184200001 ()2-s2.0-85175849086 (Scopus ID)
Funder
Swedish Research Council Formas, 2021-00877Swedish Energy Agency, 50620-1
Available from: 2023-11-28 Created: 2023-11-28 Last updated: 2025-04-24Bibliographically approved
Li, G., Boulanger, N., Iakunkov, A., Xue, H., Li, J., Tucoulou, R. & Talyzin, A. V. (2024). In operando study of microsupercapacitors with gel electrolytes using nano-beam synchrotron X-ray diffraction. Batteries & Supercaps, 7(8), Article ID e202400092.
Open this publication in new window or tab >>In operando study of microsupercapacitors with gel electrolytes using nano-beam synchrotron X-ray diffraction
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2024 (English)In: Batteries & Supercaps, E-ISSN 2566-6223, Vol. 7, no 8, article id e202400092Article in journal (Refereed) Published
Abstract [en]

Synchrotron radiation X-ray diffraction (XRD) with nanoscale beam size was used here for in situ and in operando study of micro-supercapacitors (MSC) with gel electrolyte and MXene Ti3C2Tx electrodes. The electrode structure was characterized as a function of applied voltage and distance from the gap separating electrodes using microscopic cells with cylindrical shape designed for transmission mode XRD. The devices with gel electrolytes based on H2SO4 (with H2O/PVA and DMSO/PVA) showed stable performance with no changes in MXene structure under voltage swaps between positive and negative values. Experiments with KI-based electrolytes demonstrated changes of MXene structure correlated with decrease of energy storage parameters under conditions of increased operation voltage starting from 0.8 V. The optimal performance of the MSCs was observed when the MXene structure remained unchanged upon switching the applied voltage polarity. The changes of inter-layer distance of MXene upon swap of applied voltage correlate with decrease of device performance and are undesirable for stable operation of MSC's. We also tested feasibility of X-ray fluorescence (XRF) for characterization of electrolyte ion migration in MSCs using 2D element mapping. Irreversible sorption of iodine by MXene was found using XRF mapping of charged electrodes using standard in-plane MSC device and KI electrolyte.

Place, publisher, year, edition, pages
Wiley-VCH Verlagsgesellschaft, 2024
Keywords
in operando, in situ, MXene, supercapacitor, XRD
National Category
Materials Chemistry Condensed Matter Physics
Identifiers
urn:nbn:se:umu:diva-227999 (URN)10.1002/batt.202400092 (DOI)001271189000001 ()2-s2.0-85198544521 (Scopus ID)
Funder
EU, Horizon 2020, 881603Swedish Energy Agency, 50620-1
Available from: 2024-07-24 Created: 2024-07-24 Last updated: 2024-08-20Bibliographically approved
Gurzęda, B., Boulanger, N., Enache, L.-B., Enachescu, M. & Talyzin, A. V. (2024). Microporous hydrophilic super-oxidized carbons with high surface area for removal of copper ions. Microporous and Mesoporous Materials, 378, Article ID 113259.
Open this publication in new window or tab >>Microporous hydrophilic super-oxidized carbons with high surface area for removal of copper ions
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2024 (English)In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 378, article id 113259Article in journal (Refereed) Published
Abstract [en]

Super-oxidized porous carbons produced from reduced graphene oxide have been demonstrated recently to show unique sorption properties. Here we report experiments with identical oxidative treatment applied to four very different types of porous carbon materials with extremely broad range of specific surface area (SSA) ∼350–3400 m2g−1. It is demonstrated that KOH-activated carbons can be oxidized to the same degree as graphene oxide (GO) while preserving a larger part of SSA. Prolonged oxidation with ammonium persulfate resulted in extraordinary high degree of oxidation with C/O ratio reaching 2.1. Precursor carbons with largest share of micropores are found to be more stable against oxidative treatment, while single-walled carbon nanotubes (SWCNT's) are oxidized to much less extent. While mesopores collapse, micropores survive strong oxidation treatment providing materials with rather narrow pore size distribution and high (for given oxidation degree) BET SSA up to ∼1150 m2g−1. Super-oxidized porous carbons (SOPC's) show a high abundance of hydroxyl, epoxide, carbonyl, and carboxyl functional groups (similar to GO). As a result of oxidation, the hydrophobic carbons are converted into hydrophilic materials. Characterization shows that many properties of SOPC (e.g. degree of oxidation, type of functional groups, thermal stability etc.) are rather similar to GO, except for three-dimensional porous structure which can be considered an advantage for sorbent applications. SOPC's demonstrate superior sorption capacity for Cu(II) (up to ∼105 mgg−1), which is 8-fold higher than the value for non-oxidized precursor.

Place, publisher, year, edition, pages
Elsevier, 2024
Keywords
Adsorbent, Chemical modification, Copper sorption, Porous carbon
National Category
Materials Chemistry Other Physics Topics
Identifiers
urn:nbn:se:umu:diva-228131 (URN)10.1016/j.micromeso.2024.113259 (DOI)001282466200001 ()2-s2.0-85199429465 (Scopus ID)
Funder
Swedish Energy Agency, 50620-1ÅForsk (Ångpanneföreningen's Foundation for Research and Development), N 23-275The Kempe Foundations
Available from: 2024-08-05 Created: 2024-08-05 Last updated: 2025-04-24Bibliographically approved
Nordenström, A., Boulanger, N., Vorobiev, A., Amidani, L., Bauters, S., Galanzew, J., . . . Talyzin, A. V. (2024). Neutron reflectivity for testing graphene oxide films sorption of EuCl3 in ethanol solution. Physica status solidi. B, Basic research, 261(6), Article ID 2400069.
Open this publication in new window or tab >>Neutron reflectivity for testing graphene oxide films sorption of EuCl3 in ethanol solution
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2024 (English)In: Physica status solidi. B, Basic research, ISSN 0370-1972, E-ISSN 1521-3951, Vol. 261, no 6, article id 2400069Article in journal (Refereed) Published
Abstract [en]

Neutron reflectivity (NR) was used to study the sorption of Eu(III) by graphene oxide (GO) films exposed to ethanol solution of EuCl3. Most of the earlier sorption studies have been performed using GO dispersed in solution. In contrast, layered structure of GO films imposes limitations for penetration of ions between individual sheets. The analysis of NR data recorded before and after sorption under vacuum demonstrates an increase of GO film thickness due to sorption by 35–40%. The characterization of chemical state of Eu(III) sorbed by GO films by X-ray absorption near-edge structure (XANES) in high-energy resolution fluorescence detection (HERFD) method at the Eu L3 edge reveals that it remains the same as in anhydrous EuCl3. Analysis of all collected data including reference experiments with bulk GO samples allows to conclude that EuCl3 penetrates into GO interlayers with ethanol solution and remains trapped in interlayers after evaporation of ethanol. Sorption of EuCl3 results in nearly complete amorphization of film and likely formation of voids, thus making NR models based on specific volume of unit cell not valid for quantitative evaluation of Eu sorption. Limitations of NR method must be taken into account in future studies of sorption by thin films.

Place, publisher, year, edition, pages
John Wiley & Sons, 2024
Keywords
graphene oxides, lanthanides, neutron reflectivities
National Category
Condensed Matter Physics Materials Chemistry
Identifiers
urn:nbn:se:umu:diva-223479 (URN)10.1002/pssb.202400069 (DOI)001199666100001 ()2-s2.0-85189887182 (Scopus ID)
Funder
Swedish Energy Agency, 50620-1ÅForsk (Ångpanneföreningen's Foundation for Research and Development), 23-275
Available from: 2024-04-19 Created: 2024-04-19 Last updated: 2024-06-25Bibliographically approved
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ORCID iD: ORCID iD iconorcid.org/0000-0002-3881-6764

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