Resultados totales (Incluyendo duplicados): 35619
Encontrada(s) 3562 página(s)
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355200
Dataset. 2023

ATLANTIC COD INDIVIDUAL SPATIAL BEHAVIOUR AND STABLE ISOTOPE ASSOCIATIONS IN A NO-TAKE MARINE RESERVE [DATASET]

  • Monk, Christopher
  • Power, Michael
  • Freitas, Carla
  • Harrison, Philip
  • Heupel, Michelle
  • Kuparinen, Anna
  • Moland, Even
  • Simpfendorfer, Colin
  • Villegas-Ríos, David
  • Olsen, Esben Moland
This dataset contains all data used in the analysis for the associated manuscript, as well as an R script which can be used to replicate the analysis.-- There are six files, including multispecies stable isotope data, cod sampling data, cod specific stable isotope data, cod meta data, cod positions and an R script for analysis, Foraging is a behavioural process and, therefore, individual behaviour and diet are theorized to covary. However, few comparisons of individual behaviour type and diet exist in the wild. We tested whether behaviour type and diet covary in a protected population of Atlantic cod, Gadus morhua. Working in a no-take marine reserve, we could collect data on natural behavioural variation and diet choice with minimal anthropogenic disturbance. We inferred behaviour using acoustic telemetry and diet from stable isotope compositions (expressed as δ13C and δ15N values). We further investigated whether behaviour and diet could have survival costs. We found cod with shorter diel vertical migration distances fed at higher trophic levels. Cod δ13C and δ15N values scaled positively with body size. Neither behaviour nor diet predicted survival, indicating phenotypic diversity is maintained without survival costs for cod in a protected ecosystem. The links between diet and diel vertical migration highlight that future work is needed to understand whether the shifts in this behaviour during environmental change (e.g. fishing or climate), could lead to trophic cascades, The Research Council of Norway, Award: CODSIZE 294926; Natural Sciences and Engineering Research Council; European Commission, Award: 793627; Spanish National Research Council, IF_ERC; Academy of Finland, Award: 317495; European Research Council, Award: 770884, file: cod_stable_isotopes.rdata; description: Cod specific stable isotopes data in the .rdata format.-- file: TVE2011Effort.csv; description: Sampling effort and locations in the Tvedestrand fjord.-- file: SI.rdata; description: stable isotope samples collected throughout the Tvedestrand foodweb.-- file: telem.rdata; description: Data collected during each cod sampling event, including recaptures.-- file: Allcodpositions.rdata; description: dataset "pos" contains a list of all cod positions used in the stable isotope anaylsis, Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355200
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355200
HANDLE: http://hdl.handle.net/10261/355200
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355200
PMID: http://hdl.handle.net/10261/355200
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355200
Ver en: http://hdl.handle.net/10261/355200
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355200

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355349
Dataset. 2024

EVALUACIÓN DE LA NOCHE EUROPEA DE L@S INVESTIGADOR@S ANDALUCÍA. OPEN RESEARCHERS 2023

EVALUATION OF THE EUROPEAN RESEARCHERS' NIGHT IN ANDALUSIA. OPEN RESEARCHERS 2023

  • Domínguez Álvarez, Juan Antonio
  • Lafuente, Regina
  • Ranchal Romero, Julia
  • Trujillo Carmona, Manuel
[Descripción de los métodos utilizados para la recopilación/generación de datos] La evaluación de La Noche se realiza desde 2014 a través de una encuesta dirigida a asistentes e investigadores/as Para cada colectivo se ha diseñado un cuestionario específico, aunque algunas cuestiones son comunes. Ambos cuestionarios se han alojado en la web nocheinvestiga.es desarrollada íntegramente por IESA CSIC garantizando así la privacidad, seguridad y calidad de los datos. El contenido del cuestionario se ha mantenido durante todas las ediciones, si bien la técnica de recogida de datos se ha adaptado al tipo de actividad evaluada y los recursos disponibles. En el caso de los/as participantes distinguimos a continuación tres vías para recoger los cuestionarios según el tipo de actividad en el que han participado. - Micro-encuentros: se trata de aquellas actividades dirigidas a un número limitado de personas (microcharlas talleres, visitas guiadas, etc.) en las que los participantes facilitaron una dirección de correo electrónico para reservar plaza. A esa dirección se envió una invitación que da acceso online a la encuesta para evaluar la actividad. Entre el 5 y el 23 de octubre de 2023 se enviaron 1.202 invitaciones, con 3 recordatorios de respuesta, logrando una tasa de colaboración del 31,4% lo que se traduce en 371 cuestionarios. - Gran evento del 29 de septiembre: a los espacios que han concentrado gran cantidad de talleres y actividades durante La Noche del 29 de septiembre y han tenido más afluencia de público, se desplazó un equipo de encuestadores profesionales (2 por ciudad) que entrevistaron a 885 asistentes. - Actividades virtuales: la ficha explicativa de los vídeos alojados en la página web lanochedelosinvestiadores.es incluye un enlace a la encuesta online. Sin embargo, la colaboración de los asistentes por esta vía ha sido muy escasa y se han recogido solo 6 cuestionarios. En total, La Noche ha sido evaluada por 1.262 participantes de las ocho provincias andaluzas y por 1.334 investigadores e investigadoras pertenecientes a todas las instituciones que conforman el consorcio y a otras instituciones colaboradoras., [Modalidades de tratamiento de los datos] La grabación de datos es automática. En la depuración de los datos se han eliminado los casos que no habían cumplimentado el 75% del cuestionario, los casos con una duración de cumplimentación inferior a 2 minutos, los casos cumplimentados fuera Andalucía, Ceuta y Melilla. También se han eliminado los casos de participantes menores de 14 años en cumplimiento de la Ley 3/2018, de 5 de diciembre, de Protección de Datos Personales y garantía de los derechos digitales., El libro de códigos está disponible en español y en traducción al inglés., [ES] La Noche Europea de los Investigadores es un proyecto de divulgación científica en el que los investigadores/as muestran su trabajo a los ciudadanos de una forma lúdica así como su repercusión en la vida cotidiana. Se trata de una acción Marie Sklodowska Curie (MSCA), dentro del Programa Marco de Investigación e Innovación de la UE Horizonte Europa (2021-2027). Este evento se celebra simultáneamente en casi 400 ciudades europeas de 30 países desde 2005. En las ocho capitales andaluzas han participado más de 89.000 personas en las actividades realizadas en 2023 por más de 3.000 investigadores de las universidades públicas andaluzas y de los institutos del CSIC ubicados en la región. La evaluación de la Noche Europea de los Investigadores en Andalucía se ha realizado a través de una encuesta dirigida tanto a investigadores como al público en general. En total, han valorado el evento 1.262 asistentes y 1.334 investigadores/as., [EN] The European Researchers' Night is a public science outreach event, which displays the diversity of science and its impact on citizens' daily lives in fun, inspiring ways. It is a Marie Sklodowska Curie (MSCA) action, under the EU Framework Programme for Research and Innovation Horizon Europe (2021-2027). This event that takes place simultaneously in almost 400 European cities in 30 countries and has been held since 2005. In 2023, 89.000 visitors attended these events in the eight Andalusian cities. In addition, 3.000 researchers from Andalusian public universities and CSIC institutes located in the region have participated. The evaluation of The European Researchers' Night in Andalusia was carried out through a survey addressed to both researchers and the general public. In total, 1.262 attendees and 1.334 researchers evaluated the event., Proyecto financiado por el Programa Marco de Investigación Horizon Europe de la Comisión Europea, en el marco de las acciones Marie Sktodowska-Curie., Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355349, https://doi.org/10.20350/digitalCSIC/16254
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355349
HANDLE: http://hdl.handle.net/10261/355349, https://doi.org/10.20350/digitalCSIC/16254
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355349
PMID: http://hdl.handle.net/10261/355349, https://doi.org/10.20350/digitalCSIC/16254
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355349
Ver en: http://hdl.handle.net/10261/355349, https://doi.org/10.20350/digitalCSIC/16254
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355349

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355394
Dataset. 2023

NMR SPECTROSCOPIC IDENTIFICATION OF UROLITHIN G, A NOVEL TRIHYDROXY UROLITHIN PRODUCED BY HUMAN INTESTINAL ENTEROCLOSTER SPECIES. SUPPORTING INFORMATION

  • Beltrán Riquelme, David
  • Frutos-Lisón, M.D.
  • García-Villalba, Rocío
  • Yuste, Jose E.
  • García-Aparicio, Víctor
  • Espín de Gea, Juan Carlos
  • Selma, María Victoria
  • Tomás Barberán, Francisco
Figure S1. 1H NMR spectra of urolithin D, urolithin C, urolithin M7, urolithin G, urolithin A, and isourolithin A in AcN-d3 and in DMSO-d6. *Signals from hydroxyl protons; Figure S2. 13C NMR spectrum (zoom from d = 110–115 ppm) of urolithin G in AcN-d3 and DMSO-d6. C2 and C7 were clearly separated in AcN-d3, while they appeared very close in the DMSO-d6 spectrum, Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355394
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355394
HANDLE: http://hdl.handle.net/10261/355394
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355394
PMID: http://hdl.handle.net/10261/355394
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355394
Ver en: http://hdl.handle.net/10261/355394
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355394

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355403
Dataset. 2023

GLOBAL OCEAN DATA ANALYSIS PROJECT VERSION 2.2023 (GLODAPV2.2023)

  • Lauvset, Siv K.
  • Lange, Nico
  • Tanhua, Toste
  • Bittig, Henry C.
  • Olsen, Are
  • Kozyr, Alex
  • Álvarez-Rodríguez, Marta
  • Azetsu-Scott, Kumiko
  • Becker, Susan
  • Brown, Peter J.
  • Carter, Brendan R.
  • Cotrim da Cunha, Leticia
  • Feely, Richard A.
  • Hoppema, Mario
  • Humphreys, Matthew P.
  • Ishii, Masao
  • Jeansson, Emil
  • Jones, Steve D.
  • Lo Monaco, Claire
  • Murata, Akihiko
  • Müller, Jens Daniel
  • Pérez, Fiz F.
  • Schirnick, Carsten
  • Steinfeldt, Reiner
  • Suzuki, Toru
  • Tilbrook, Bronte
  • Ulfsbo, Adam
  • Velo, A.
  • Woosley, Ryan J.
  • Key, Robert M.
12 files, This dataset consists of the GLODAPv2.2023 data product composed of data from 1108 scientific cruises covering the global ocean between 1972 and 2021. It includes full depth discrete bottle measurements of salinity, oxygen, nitrate, silicate, phosphate, dissolved inorganic carbon (TCO2), total alkalinity (TAlk), CO2 fugacity (fCO2), pH, chlorofluorocarbons (CFC-11, CFC-12, CFC-113, and CCl4), SF6, and various isotopes and organic compounds. It was created by appending data from 23 cruises to GLODAPv2.2022 (Lauvset et al., 2022, NCEI Accession 0257247). The data for salinity, oxygen, nitrate, silicate, phosphate, TCO2, TAlk, pH, CFC-11, CFC-12, CFC-113, CCl4, and SF6 were subjected to primary and secondary quality control. Severe biases in these data have been corrected for, and outliers removed. However, differences in data related to any known or likely time trends or variations have not been corrected for. These data are believed to be accurate to 0.005 in salinity, 1% in oxygen, 2% in nitrate, 2% in silicate, 2% in phosphate, 4 µmol kg-1 in TCO2, 4 µmol kg-1 in TAlk, and for the halogenated transient tracers and SF6: 5%, Funding Information: DOE, NOAA, NSF, EU agencies, Japan Climate Research Program, Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355403
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355403
HANDLE: http://hdl.handle.net/10261/355403
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355403
PMID: http://hdl.handle.net/10261/355403
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355403
Ver en: http://hdl.handle.net/10261/355403
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355403

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355410
Dataset. 2024

WETYDAS: WEATHER TYPES DATASET IN SPANISH MAINLAND, V.1.1.0. [DATASET]

TIPOS DE TIEMPO EN ESPAÑA (1950-2023)

  • Cortesi, Nicola
  • Peña Angulo, Dhais
[EN] WETYDAS contains 12 TXT archives localized by their coordinates in NCAR grid; information include year, month, day and code of weathee type. [ES] WETYDAS consta de 12 archivos formato TXT geolocalizados por sus coordenadas en la malla NCAR; la información incluye el año, mes y día, así como el código del tipo de tiempo resultante., [EN] It has been applied the Jenkinson & Collison classification of Weather Types to Iberian Peninsula and Balearic Island by using the daily NCAR-NCEP grid surface pressure dataset (January-1950/December-2023). Grid resolution/2.5ºx2.5 lat/long) produces 12 series. Weather Types classification includes 8 directional pure, Anticyclonic and Cyclonic pure types, and combination of previous ones in the hybrid types. Non determines cases were spread homogeneously., [ES] Se ha aplicado la clasificación de tipos de tiempo (Weather Types) de Jenkinson y Collison a la malla de presiones diaria del reanálisis NCAR-NCEP (periodo Enero 1950-Diciembre 2023) correspondiente a la Península Ibérica y Baleares. Por la resolución de dicha malla (2.5º x 2.5º lat/long) el total de nodos de control es de 12. Los tipos de tiempo resultantes incluyen los 8 direccionales puros, Anticiclónico y Ciclónico puro, y la combinación de 8 tipos híbridos entre las categorías previas. Los casos indeterminados fueron distribuidos proporcionalmente entre las clases previas., No

Proyecto: //
DOI: http://hdl.handle.net/10261/355410, https://doi.org/10.20350/digitalCSIC/16255
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355410
HANDLE: http://hdl.handle.net/10261/355410, https://doi.org/10.20350/digitalCSIC/16255
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355410
PMID: http://hdl.handle.net/10261/355410, https://doi.org/10.20350/digitalCSIC/16255
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355410
Ver en: http://hdl.handle.net/10261/355410, https://doi.org/10.20350/digitalCSIC/16255
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355410

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355492
Dataset. 2023

IDENTIFYING NATURAL BIOACTIVE PEPTIDES FROM THE INK BY-PRODUCT OF COMMON OCTOPUS (OCTOPUS VULGARIS) USING PROTEOMICS

  • Gestal, C.
  • Carrera, Mónica
  • Dios, S.
10 files, f.MSV000089896/ccms_parameters/params.xml; f.MSV000089896/ccms_result/MCMMCM34021201_02_03_INK_BATCH_FDR_UNIGENE_PULPO_plus_Cephalopoda_Percolator.mzTab; f.MSV000089896/ccms_statistics/statistics.tsv; f.MSV000089896/peak/MCMMCM34021201.mzML; f.MSV000089896/peak/MCMMCM34021202.mzML; f.MSV000089896/peak/MCMMCM34021203.mzML; f.MSV000089896/raw/MCMMCM34021201.raw; f.MSV000089896/raw/MCMMCM34021202.raw; f.MSV000089896/raw/MCMMCM34021203.raw; f.MSV000089896/result/MCMMCM34021201_02_03_INK_BATCH_FDR_UNIGENE_PULPO_plus_Cephalopoda_Percolator.mzTab, Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355492
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355492
HANDLE: http://hdl.handle.net/10261/355492
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355492
PMID: http://hdl.handle.net/10261/355492
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355492
Ver en: http://hdl.handle.net/10261/355492
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355492

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355514
Dataset. 2024

SUPPLEMENTARY INFORMATION - SPATIAL AND SEASONAL VARIABILITY OF PICOPLANKTON ABUNDANCE AND GROWTH RATES IN THE SOUTHERN BAY OF BISCAY

  • de la Iglesia-Vélez, Braulio
  • Díaz-Pérez, Laura
  • Acuña Fernández, José Luis
  • Morán, Xosé Anxelu G.
7 páginas, 1 tabla, 5 figuras, Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355514
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355514
HANDLE: http://hdl.handle.net/10261/355514
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355514
PMID: http://hdl.handle.net/10261/355514
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355514
Ver en: http://hdl.handle.net/10261/355514
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oai:digital.csic.es:10261/355514

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355518
Dataset. 2024

APPENDIX A. SUPPLEMENTARY DATA: A COMPARATIVE STUDY OF THE DIGESTION BEHAVIOR AND FUNCTIONALITY OF PROTEIN FROM CHIA (SALVIA HISPANICA L.) INGREDIENTS AND PROTEIN FRACTIONS

  • Wang, Yan
  • Hernández-Álvarez, Alan Javier
  • Goycoolea, Francisco M.
  • Martínez-Villaluenga, Cristina
Figure 1S. Comparison of total protein content in undigested Mexican and British chia (Salvia hispanica L.) ingredients and protein fractions. Abbreviations: DDF, degummed-defatted chia flour; PC, protein concentrate; Alb, albumin; Glo, globulin. Different lowercase letter within each sample group indicates statistical differences among the same chia samples from different locations (p < 0.05, Tukey test). Figure 2S. SEC profile at 214 nm for undigested Mexican and British chia (Salvia hispanica L.) samples and their digestates after gastric and intestinal digestion. A) degummed-defatted flour; B) protein concentrate; C) albumin, D) globulin. Abbreviations: M, Mexican chia samples; B, British chia samples; U, undigested; G, gastric phase; I, intestinal phase. Figure 3S. Kinetic evaluation of ROS production in Caco-2 cells and RAW264.7 macrophages in the presence of Mexican and British chia samples. A) ROS of Mexican chia samples in RAW264.7 Macrophages, B) ROS of British chia samples in RAW264.7 Macrophages, C) ROS of Mexican chia samples in Caco-2 cells D) ROS of British chia samples in Caco-2 cells. Abbreviations: DDF, degummed-defatted chia flour; PC, protein concentrate; Alb, albumin; Glo, globulin; M, Mexican chia samples; B, British chia samples., Table 1S. Peptide molecular weight distribution of chia (Salvia hispanica L.) samples and digestates., Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355518
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355518
HANDLE: http://hdl.handle.net/10261/355518
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355518
PMID: http://hdl.handle.net/10261/355518
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355518
Ver en: http://hdl.handle.net/10261/355518
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oai:digital.csic.es:10261/355518

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355698
Dataset. 2023

OCTOPOD HOX GENES AND CEPHALOPOD PLESIOMORPHIES [DATASET]

  • Barrera Grijalba, Cristian Camilo
  • Rodríguez Monje, Sonia Victoria
  • Gestal, C.
  • Wollesen, Tim
2 assembled transcriptomes and the respective raw reads: “Ovu1”: mRNA of almost hatched individuals (stage XX) and “Ovu2”: pooled mRNA of developmental stages VIII, XI, XV, XVIII, RNA-seq libraries were constructed with a Lexogen SENSE mRNA-Seq Library Prep Kit V2 and sequenced with an Illumina Hi-Seq 2500 generating paired-end, stranded 125 bp libraries resulting in 53,523,481 (ovu1) and 63,328,653 (ovu2) paired end reads. The overall transcriptome assembly follows the procedure performed by De Oliveira et al. (2016) [42]. The short‐read libraries were preprocessed using Trimmomatic v. 0.36 (ref. [43]) to remove known specific Illumina adapters from the paired‐end libraries (Illumina universal adapter). Filtering by quality and length was performed with a SLIDINGWINDOW:4:15 MINLEN:36. First and last nucleotides from reads with low quality score were clipped and the library file was converted into FASTA format using fq2fa from SeqKit version 0.11.0 (ref. [44]). Quality of the initial and filtered library was assessed with the software FastQC v.0.11.8 (ref. [45]) considering quality score of the bases, GC‐content, and read length. 13.33% (ovu1) and 16,23% (ovu2) of reads were excluded during the preprocessing procedure resulting in a total of 46,386,109 (ovu1) and 53,052,713 (ovu2) reads. The assemblies and all downstream analyses were conducted with a high‐quality and clean library. The filtered transcriptome was assembled into contiguous cDNA sequences with IDBA_tran v1.1.3 software (ref. [46]) using the default settings (except: −mink20 −maxk 80 −step5). The resulting assembly was assessed using the tool QUAST (available at: http://quast.bioinf.spbau.ru [47]). The number of contigs was 16,723 sequences (ovu1) and 18,551 (ovu2), Peer reviewed

Proyecto: //
DOI: http://hdl.handle.net/10261/355698
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355698
HANDLE: http://hdl.handle.net/10261/355698
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355698
PMID: http://hdl.handle.net/10261/355698
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355698
Ver en: http://hdl.handle.net/10261/355698
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355698

Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355708
Dataset. 2024

SUPPLEMENTARY MATERIALS FOR POLY(VINYL BENZOATE)-B-POLY(DIALLYLDIMETHYL AMMONIUM TFSI)-B-POLY(VINYL BENZOATE) TRIBLOCK COPOLYMER ELECTROLYTES FOR SODIUM BATTERIES [DATASET]

  • Stigliano, Pierre L.
  • Gallastegui, Antonela
  • Villacis Segovia, Carlos
  • Amores, Marco
  • Kumar, Ajit
  • O'Dell, Luke A.
  • Fang, Jian
  • Mecerreyes, David
  • Pozo Gonzalo, Cristina
  • Forsyth, Maria
Experimental Section: Materials: Sodium bis(fluorosulfonyl)imide (NaFSI) (Solvionic, 99.99% purity was dried at 50 °C on under vacuum overnight and stored in Ar filled glovebox. The polymer electrolyte membranes were prepared as shown in Figure 3, NaFSI and the block copolymer were dissolved in a solvent mixture of tetrahydrofuran (THF) and acetonitrile (ACN). The solution was stirred at RT overnight and then cast on Teflon mold for solvent evaporation. The dry membranes were hot pressed and then dry at RT under vacuum, before being stored in Ar filled glovebox. Synthesis of PVB-PDADMTFSI-PVB block copolymers: The initial step of the synthesis involved synthesizing the double-functionalized chain transfer agent (CTA), known as X-DiEST-X. Diethyl meso-2,5-dibromoadipate (10 g; 27.7 mmol) was dissolved in 250 mL of 96% ethanol (EtOH) at room temperature in a 500 mL round bottom flask. Subsequently, potassium ethyl xanthogenate was added to the solution and stirred for 90 minutes. The reaction took place at room temperature for 4 hours. Upon completion, the resulting potassium bromide salt was filtered, and ethanol was removed under vacuum. The product was then dissolved in dichloromethane (DCM) and washed three times with distilled water. After evaporating the DCM, the product was dried under vacuum for 24 hours. The second step involved synthesizing the MacroCTA, denoted as X-PAm-DiEst-PAm-X, to achieve water solubility, a crucial property for the polymerization of PDADMACl. X-DiEst-X (4 g), acrylamide (12.8 g), and radical initiator AIBA (0.098 g) were dissolved in 8 mL of water and 35 mL of ethanol in a 50 mL Schlenk flask. The solution was then deoxygenated using nitrogen for 30 minutes. The reaction proceeded for one hour until a white precipitate formed. The precipitate was subsequently extracted and dried under vacuum at 40 °C overnight. Finally, the product was characterized using 1H-NMR and MALDI-TOF techniques (Figures S1 and S2). The polymerization process of the PDAMDATFSI block consisted of two stages. The first stage involved synthesizing poly-DADMACl: X-PAm-DiEst-PAm-X (2 g), AIBA (0.088 g), and PDADMACl (15.6 mL, 65 wt% aqueous solution) in a 50 mL Schlenk tube. The mixture was stirred and degassed with nitrogen for 30 minutes. The reactor was then placed in a preheated oil bath set at 60 °C. The final polymer was precipitated using a 1:1 mixture of ethanol and acetone, followed by filtration and vacuum drying at 40 °C. The product was analyzed using 1H-NMR in D2O (Figure S3). Once the PDADMACl polymer was obtained, an anion exchange was conducted to yield PDADMATFSI. PDADMACl was dissolved in distilled water and slowly added to a solution containing LiTFSI and distilled water under magnetic stirring. The resulting precipitate was then separated from the solvent, dried under vacuum at 40 °C overnight, and subsequently characterized using GPC-SEC (Figure S4). Two chain lengths of PDADMATFSI were investigated in this work: 33K and 17.5K, as shown in Table 1 To obtain the final product, PVB-b-PDADMATFSI-b-PVB triblock copolymers, PDADMATFSI and vinyl benzoate were dissolved in dimethylformamide (DMF) with AIBN as the initiator. The solution was deoxygenated with nitrogen for 30 minutes and then immersed in a preheated oil bath at 65 °C. After 24 hours of reaction, the final polymer was precipitated in cold ethanol, dried under vacuum at 40 °C for 24 hours, and the structure was characterized through 1H-NMR (Figure S5-8). MALDI-TOF: For MALDI-TOF measurements a Bruker Autoflex Speed system (Bruker, Germany) integrated with a Smartbeam-II laser (Nd:YAG, 355nm, 2 kHz) was used, with laser power adjusted during the measurements. The spectrum was acquired in linear mode with an average of 5000 shots. Samples were mixed in MeOH at a concentration of 10 mg/mL. The matrix used was 2,5-DHB, dissolved in MeOH at a concentration of 20 mg/mL. NaTFA was the cation donor (10 mg/mL dissolved in MeOH). A matrix/polymer/salt solution with 10:5:1 ratio was used and 0.5 μL were hand-spotted on the ground steel target plate. Gas Permeation Chromatography (GPC): For GPC a 1200 Infinity gel permeation chromatograph (GPC, Agilent Technologies) integrated with IR detector, a PLgel 5 mm MIXED-D column and a PLgel guard column (Agilent Technologies) was used. As eluent a 0,1 M LiTFSI/DMF solution was used and flow rate was set at 1.0 mL min-1 at 50 oC. PMMA standards (Agilent Technologies, Mp = 0.55 - 1568 x103) were used to perform calibration. Differential Scanning Calorimetry (DSC): Thermal properties of the neat block copolymers and polymer electrolyte membranes were measured by Netzsch DSC (214Polyma). All samples were characterized in the range of -100 and 150 oC, with a heating rate of 40K/min. The second heating is reported. Fourier Transform Infrared Spectroscopy (FTIR): The samples were measured by a Perkin Elmer instrument using a single diamond attenuated reflection unit. The spectra were measured in the region from 4000 to 650 cm-1. Transmission Electron Microscopy (TEM): Block copolymer films were placed into freshly prepared Procure 812 resin (ProSciTech Kirwan, QLD, C045) for 2 hours under vacuum infiltration at RT. The samples were then removed and put in resin mold (Procure 812 resin) before curing for 3 days at 580C. The resin block was sectioned using a Leica UC7 ultramicrotome to obtain silver interference (~50nm) sections and collected onto EMSFCFTH 400 mesh copper grids (ProSciTech Kirwan, QLD). Samples were imaged using a Tecnai 12 Transmission Electron Microscope (FEI, Eindhoven, The Netherlands), operating voltage of 120 kV. At all times low dose procedures were followed, using an electron dose of less than 5 electrons/Å2 for all imaging. Images were recorded using a FEI Eagle 4k x 4k CCD camera at a range of magnifications using AnalySIS v3.2 camera control software (Olympus). Solid State Magic Angle Spin Nuclear Magnetic Resonance Spectroscopy (MAS-NMR): For NMR spectroscopy, a Bruker Avance III 500 MHz ultra shield wide bore spectrometer was used. Zirconia MAS NMR rotors (diameter: 1.3 mm) were filled with samples inside Ar filled glovebox. Spectra were analysed using TopSpin software. Full-width half-maximum (fwhm) values were calculated by fitting the peaks with Gaussian/Lorentzian function. Ionic Conductivity: Ionic conductivity was measured using MTZ-35 in the frequency range of 1 Hz to 10 MHz (amplitude of 0.01 V) in the temperature range of 30 and 90 °C. The polymer electrolyte membranes were cut into 12 mm diameter round discs and andwiched between two stainless steel electrodes inside of a coin cell. The coin cell was then put in a custom-built barrel cell. All the spectra were fitted by MTlab software. Electrochemical Characterization: TNa + at 70 oC was measured with the Bruce−Vincent method, the equation used for calculation is: TNa+ = 𝐼s(Δ𝑉 − 𝐼0𝑅i0)/𝐼0(Δ𝑉 − 𝐼s𝑅is) Where ΔV = applied constant potential, I0 and Is = initial and steady-state currents, respectively, and Rio and Ris = initial and steady state interfacial resistance, respectively. Na|Na symmetric cell cycling was performed using a coin cell with the electrolyte membrane (thickness 300 μm, diameter 14 mm) sandwiched between 2 Na metal discs (diameter 10 mm). Cells were assembled inside an Ar filled glovebox. Na-metal stripping and plating were studied at different currents using a Biologic VMP3 potentiostat, data were processed with EC-Lab software. A homemade 2-electrode Swagelok-type cell was employed for Sodium-Air Battery (SAB) testing. The cell parts were dried at 60 °C overnight and then transferred to an Ar filled glovebox for assembling. The SAB cell was composed of a sodium metal disk (diameter = 12 mm, Sigma Aldrich), the polymer electrolyte membrane (diameter = 12.7 mm) and multi-doped carbon nanofibers air cathode (reported in literature). The surface of the air cathode was wetted with 50 uL of liquid electrolyte (NaTFSI:diglyme:C4mpyrTFSI in mol ratio 1:4:1) to improve contact between air cathode and polymer electrolyte membrane. Once assembled, the cells were taken outside of the Ar filled glovebox and pressurized under pure oxygen (99.99% purity). The cells were left to rest for 8 h at open circuit voltage and 50 oC. Subsequently, a current density of -75 μA cm-2 was applied, with a cut-off potential of 1.6 V.-- Under a Creative Commons license CC BY 4.0 Deed Attribution 4.0 International, Experimental Section, Figure S1: H-NMR (300 MHz) di funcional CTA X-PAm-DiEst-PAm-X in D2O; Figure S2: MALDI-TOF analysis of X-Pam-DiEst-Pam-X (X-AdA-X); Figure S3: H NMR (300 MHz) of MacroCTA in D2O; Figure S4 H-NMR of PVB11.5K–b–PDADMATFSI33K–b–PVB11.5K; Figure S5 H-NMR of PVB11.5K–b–PDADMATFSI17.5K–b–PVB11.5K; Figure S6 H-NMR of PVB22.5K–b–PDADMATFSI33K–b–PVB22.5K; Figure S7 H-NMR of PVB22.5K–b–PDADMATFSI17.5K–b–PVB22.5K; Table S1: FTIR absorption band positions and assignment for neat PVB-PDADMAT-PVB BCPs; Figure S8: TEM images of BCP BCP-1233 and BCP-2218; Table S2: Sample name and characteristics of the membrane with 2:1 Na:PDADMATFSI mol ratio for all four compositions of neat polymer; Figure S9: TEM images of BCP BCP-1233-Na and BCP-2218-Na; Figure S10: Ratio between integrals of the two coordination peaks observed in 23Na NMR; Figure S11: FTIR spectra of neat BCP and BCP-NaFSI mixtures with a 2:1 Na:PDADMA mol ratio; Figure S12: Galvanostatic cycling of sodium symmetrical cells using BCP-1233-Na at 70 °C; Figure S13: Photo of the membrane after galvanostatic cycling in Na| Na cells showing the formation of large dendrites; Figure S14: SEM images of the surface of BCP-1233-Na and BCP-2218-Na, and EDS layered image zoomed on one of the structures found on the surface of BCP-2218-Na; Figure S15: SEM images of the cross-section of BCP-1233(2); Figure S16: Cell configuration of the home modified Swagelok-type Na-O2 cell used., This project received funding from the European Union’s Horizon 2020 research and innovation program under the Marie Skłodowska-Curie grant agreement No. 860403. The authors acknowledge the Australian Research Council (ARC) for funding through Discovery Programme DP160101178 and the ARC Industry Transformation Training Centre for Future Energy Technologies (storEnergy) for funding under grant agreement No. IC180100049., Peer reviewed

Proyecto: EC/H2020/860403
DOI: http://hdl.handle.net/10261/355708
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355708
HANDLE: http://hdl.handle.net/10261/355708
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355708
PMID: http://hdl.handle.net/10261/355708
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355708
Ver en: http://hdl.handle.net/10261/355708
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/355708

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