ESTRUCTURACION DE MATERIALES AVANZADOS MEDIANTE LASERES ULTRARRAPIDOS PARA APLICACIONES EN FOTONICA, SENSADO Y BIO-ACTUACION: SINTESIS, MODIFICACION Y APLICACIONES
PID2020-112770RB-C22
•
Nombre agencia financiadora Agencia Estatal de Investigación
Acrónimo agencia financiadora AEI
Programa Programa Estatal de I+D+i Orientada a los Retos de la Sociedad
Subprograma Programa Estatal de I+D+i Orientada a los Retos de la Sociedad
Convocatoria Proyectos I+D
Año convocatoria 2020
Unidad de gestión Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020
Centro beneficiario UNIVERSIDAD AUTONOMA DE MADRID
Identificador persistente http://dx.doi.org/10.13039/501100011033
Publicaciones
Found(s) 13 result(s)
Found(s) 1 page(s)
Found(s) 1 page(s)
Dataset of Mechanically stimulated gas emission from pellets of sodium alanate subjected to rubbing at room temperature under vacuum and related surface, structural, mechanical, and tribological characterization of the pellets
Digital.CSIC. Repositorio Institucional del CSIC
- Muñoz-Cortés, Esmeralda
- Ibryaeva, Olga
- Manso Silván, Miguel
- Zabala, Borja
- Flores, Eduardo
- Gutiérrez, Almudena
- Ares, José R.
- Nevshupa, Roman
The pellets were subjected to reciprocating rubbing under vacuum (10-7 mbar range) using an alumina sphere, 3 mm in diameter. A specially designed friction cell with nearly zero own gas emission was used. The motion frequency was 1 Hz. One motion cycle consisted of one forth and one back stroke, each of which lasted for about 40 ms. The indenter stood still for around 50 ms after the forth stroke and 870 ms after the back one. The stroke length was la = 7 mm, the mean sliding speed was Vs = 0.18 m s-1 and the normal load was in the range 0.22 – 0.88 N. The total and partial gas pressures were measured in the experimental vacuum chamber, where the pellets were rubbed, using an ionization Bayard-Alpert type vacuum gauge and a quadrupole mass-spectrometer, correspondingly. To quantify minute gas emission rates (<1 nmol/s) the experimental chamber was connected to a gas-expansion chamber through a diaphragm, which conductance under molecular gas flow was carefully measured. Before starting the experiments, the chamber was pumped out for at least 48 hours to achieve stable background pressure (the rate of change of low-pass filtered pressure signal ≤10-11 mbar s-1). The gas emission was evaluated from the pressure time series during the mechanical action and benchmarked against the stable background. The gas composition and the emission rates were determined using a previously developed statistical matrix method.
X-ray diffraction (XRD) with Cu Kα (λ = 0.15418 nm) radiation was employed for the structural characterization of NaAlH4. To assess the thermal stability of NaAlH4 Temperature-Programmed Desorption Mass-Spectrometry (TPD-MS) was used. A portion of NaAlH4 powder was placed into an alumina crucible in a glove box under Ar atmosphere (MBraun, <1 ppm H2O, <10 ppm O2). Alumina crucible was used instead of a Pt one to avoid possible decomposition of NaAlH4 due to the catalytic effect of Pt. The crucible was transferred to the TPD-MS system, where it was set into another Pt crucible. During the transfer, the sample was briefly exposed to the atmospheric air (about 5 min). The test was carried out under an Ar flux of 50 ml/s and a heating rate of 5 ºC/min.
The mechanically affected zones were characterized using FTIR spectrometry, Raman confocal spectroscopy (incident laser wavelength = 532 nm and power 5.6 mW) and Scanning Electron Microscopy (Hitachi S 800) to contrast possible structural and chemical variations induced in the material by the mechanical action. All the results were benchmarked against the measurements on the pristine zones of the same pellets., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal dehydrogenation of sodium alanate through the application of mechanical energy. An application of mechanical energy was explored as a new non-thermal method to drive H2 emission from undoped sodium alanate at room temperature. Dehydrogenation reactions were studied on a micrometer scale using localized rubbing under ultrahigh vacuum. Mechanically Stimulated Gas Emission Mass-Spectrometry (MSGE-MS) including the Dynamic gas expansion method was used to determine the kinetic parameters of hydrogen emission as well as the composition and emission behaviour of trace gases. It was found that mild rubbing of NaAlH4 pellets under vacuum led to intensive and almost instantaneous gas emission. The dominating species in the emitted gases was H2 (>99%). Traces (~0.1%) of mono- and polyalanes, NaAlH4 vapours, CO2 and other no identified gases were registered. Several H2 emission modes, which characteristic time constants ranged widely from 0.6 to 465 s, were observed. None of the dehydrogenation reactions involved could be connected to either the thermal effect of friction or the direct coupling of mechanical forces to the energy landscape of chemical reactions. The study was complemented by structural, morphological, tribological, mechanical and surface analyses. It was suggested that the tribochemical reactions can be triggered by plastic deformation and shearing., This study was co-funded by Spanish Ministry for Science and Innovation (grants PID2019-111063RB-I00, PID2020-112770RB-C22 and RTI2018-099794-B-I00) and the Basque Government via the EMAITEK Plus 2020 programme., 1.Dataset of mass-spectrometry time series of mechanically stimulated gas emission from sodium alanate (NaAlH4) pellets under vacuum.-- 2. Dataset of Thermal Programmed Desorption – Mass-Spectrometry (TPD-MS) analysis of sodium alanate.-- 3. Dataset of X-ray diffraction of sodium alanate.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of sodium alanate.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of sodium alanate., No
X-ray diffraction (XRD) with Cu Kα (λ = 0.15418 nm) radiation was employed for the structural characterization of NaAlH4. To assess the thermal stability of NaAlH4 Temperature-Programmed Desorption Mass-Spectrometry (TPD-MS) was used. A portion of NaAlH4 powder was placed into an alumina crucible in a glove box under Ar atmosphere (MBraun, <1 ppm H2O, <10 ppm O2). Alumina crucible was used instead of a Pt one to avoid possible decomposition of NaAlH4 due to the catalytic effect of Pt. The crucible was transferred to the TPD-MS system, where it was set into another Pt crucible. During the transfer, the sample was briefly exposed to the atmospheric air (about 5 min). The test was carried out under an Ar flux of 50 ml/s and a heating rate of 5 ºC/min.
The mechanically affected zones were characterized using FTIR spectrometry, Raman confocal spectroscopy (incident laser wavelength = 532 nm and power 5.6 mW) and Scanning Electron Microscopy (Hitachi S 800) to contrast possible structural and chemical variations induced in the material by the mechanical action. All the results were benchmarked against the measurements on the pristine zones of the same pellets., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal dehydrogenation of sodium alanate through the application of mechanical energy. An application of mechanical energy was explored as a new non-thermal method to drive H2 emission from undoped sodium alanate at room temperature. Dehydrogenation reactions were studied on a micrometer scale using localized rubbing under ultrahigh vacuum. Mechanically Stimulated Gas Emission Mass-Spectrometry (MSGE-MS) including the Dynamic gas expansion method was used to determine the kinetic parameters of hydrogen emission as well as the composition and emission behaviour of trace gases. It was found that mild rubbing of NaAlH4 pellets under vacuum led to intensive and almost instantaneous gas emission. The dominating species in the emitted gases was H2 (>99%). Traces (~0.1%) of mono- and polyalanes, NaAlH4 vapours, CO2 and other no identified gases were registered. Several H2 emission modes, which characteristic time constants ranged widely from 0.6 to 465 s, were observed. None of the dehydrogenation reactions involved could be connected to either the thermal effect of friction or the direct coupling of mechanical forces to the energy landscape of chemical reactions. The study was complemented by structural, morphological, tribological, mechanical and surface analyses. It was suggested that the tribochemical reactions can be triggered by plastic deformation and shearing., This study was co-funded by Spanish Ministry for Science and Innovation (grants PID2019-111063RB-I00, PID2020-112770RB-C22 and RTI2018-099794-B-I00) and the Basque Government via the EMAITEK Plus 2020 programme., 1.Dataset of mass-spectrometry time series of mechanically stimulated gas emission from sodium alanate (NaAlH4) pellets under vacuum.-- 2. Dataset of Thermal Programmed Desorption – Mass-Spectrometry (TPD-MS) analysis of sodium alanate.-- 3. Dataset of X-ray diffraction of sodium alanate.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of sodium alanate.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of sodium alanate., No
Tribochemically driven dehydrogenation of undoped sodium alanate under room temperature
Digital.CSIC. Repositorio Institucional del CSIC
- Muñoz-Cortés, Esmeralda
- Ibryaeva, Olga
- Manso Silván, Miguel
- Zabala, Borja
- Flores, Eduardo
- Gutiérrez, Almudena
- Ares, José R.
- Nevshupa, Roman
n application of mechanical energy was explored as a new non-thermal method to drive H2 emission from undoped sodium alanate at room temperature. It was found that mild rubbing of NaAlH4 pellets under vacuum led to intensive and almost instantaneous gas emission. The dominating species in the emitted gases was H2 (>99%). Traces of mono- and polyalanes, NaAlH4 vapours, CO2 and other non-identified gases were registered. H2 emission involved several first-order processes, whose characteristic time constants ranged widely from 0.6 to 465 s. None of the dehydrogenation reactions could be connected to either the thermal effect of friction or the direct coupling of mechanical forces to the energy landscape of chemical reactions. In turn, it was suggested that the tribochemical reactions can be triggered by plastic deformation and shearing. A linked diffusion-wear model of NaAlH4 triboinduced dehydrogenation, which consistently explains all empirical findings, was put forward., This work was financially supported by the Ministry of Science and Innovation of Spain (grants PID2019-111063RB-I00, PID2020-112770RB-C22 and RTI2018-099794-B-I00) and the Basque Government via the EMAITEK Plus 2020 programme., Peer reviewed
Surface characterization of alkane viral anchoring films prepared by titanate-assisted organosilanization
Digital.CSIC. Repositorio Institucional del CSIC
- Sanz Calderón, Aida
- Cantero, Miguel
- Pérez, Uxia
- Ortega-González, Paula
- Martin, Carmen
- Pablo, Pedro J. de
- Manso Silván, Miguel
- Hernando-Pérez, Mercedes
8 pags., 5 figs., Studies of virus adsorption on surfaces with optimized properties have attracted a lot of interest, mainly due to the influence of the surface in the retention, orientation and stability of the viral capsids. Besides, viruses in whole or in parts can be used as cages or vectors in different areas, such as biomedicine and materials science. A key requirement for virus nanocage application is their physical properties, i.e. their mechanical response and the distribution of surface charge, which determine virus-substrate interactions and stability. In the present work we show two examples of viruses exhibiting strong surface interactions on homogeneous hydrophobic surfaces. The surfaces were prepared by titanate assisted organosilanization, a sol-gel spin coating process, followed by a mild annealing step. We show by surface and interface spectroscopies that the process allows trapping triethoxy-octylsilane (OCTS) molecules, exhibiting a hydrophobic alkane rich surface finishing. Furthermore, the surfaces remain flat and behave as more efficient sorptive surfaces for virus particles than mica or graphite (HOPG). Also, we determine by atomic force microscopy (AFM) the mechanical properties of two types of viruses (human adenovirus and reovirus) and compare the results obtained on the OCTS functionalized surfaces with those obtained on mica and HOPG. Finally, the TIPT+OCTS surfaces were validated as platforms for the morphological and mechanical characterization of virus particles by using adenovirus as initial model and using HOPG and mica as standard control surfaces. Then, the same characteristics were determined on reovirus using TIPT+OCTS and HOPG, as an original contribution to the catalogue of physical properties of viral particles., This work was supported by the grant Ayudas a Proyectos de I+D para Jóvenes Doctores de la Universidad Autónoma de Madrid 2021 (SI3/PJI/2021–00216) supported by Comunidad de Madrid and Universidad Autónoma de Madrid to M.H-P. Also, M.H-P acknowledges funding from the Spanish Ministry of Science and Innovation (TED2021–129937B-I00). Grant PID2019–104098GB-I00/AEI/10.13039/501100011033, co-funded by the Spanish State Research Agency and the European Regional Development Fund to C.S.M. The CNB-CSIC was further supported by a Spanish State Research Agency Severo Ochoa Excellence grant (SEV 2017–0712). C.S.M is a member of the CSIC funded consortium LifeHub (CSIC grant number: 202120E47). REACT-EU funding by Comunidad Autónoma de Madrid is also acknowledged. M.M.S acknowledges funding from MCIN/AEI /10.13039/501100011033 (PID2020–112770RB-C22). P.J.P acknowledges projects FIS2017–89549-R; and FIS2017–90701-REDT. P.J.P also acknowledges the Human Frontiers Science Program (HFSPO RGP0012/2018)., Peer reviewed
DOI: http://hdl.handle.net/10261/288373, https://api.elsevier.com/content/abstract/scopus_id/85146151638
Process design for the manufacturing of soft X-ray gratings in single-crystal diamond by high-energy heavy-ion irradiation
Digital.CSIC. Repositorio Institucional del CSIC
- García, G.
- Martin, M
- Ynsa, M. D.
- Torres-Costa, Vicente
- Crespillo, M.L.
- Tardío, M.
- Olivares Villegas, José
- Bosia, F
- Peña-Rodríguez, O.
- Nicolás, José
- Tallarida, Massimo
Artículo con 9 figuras, This paper describes in detail a novel manufacturing process for optical gratings suitable for use in the UV and soft X-ray regimes in a single-crystal diamond substrate based on highly focused swift heavy-ion irradiation. This type of grating is extensively used in light source facilities such as synchrotrons or free electron lasers, with ever-increasing demands in terms of thermal loads, depending on beamline operational parameters and architecture. The process proposed in this paper may be a future alternative to current manufacturing techniques, providing the advantage of being applicable to single-crystal diamond substrates, with their unique properties in terms of heat conductivity and radiation hardness. The paper summarizes the physical principle used for the grating patterns produced by swift heavy-ion irradiation and provides full details for the manufacturing process for a specific grating configuration, inspired in one of the beamlines at the ALBA synchrotron light source, while stressing the most challenging points for a potential implementation. Preliminary proof-of-concept experimental results are presented, showing the practical implementation of the methodology proposed herein., The authors acknowledge funding support by the following projects: PID2020-112770RB-C22 from the Spanish Ministry of Science
and Innovation, TechnoFusión (III)-CM (S2018/EMT-4437) from Comunidad de Madrid (cofinanced by ERDF and ESF), agreement between Community
of Madrid and Universidad Autónoma de Madrid (item “Excellence of University Professorate”). M.L.C. acknowledges financial support from the research
project “Captacion de Talento UAM” Ref: #541D300 supervised by the Vice-Chancellor of Research of Universidad Autónoma de Madrid (UAM). LOREA
beamline at ALBA is a project co-funded by the European Regional Development Fund (ERDF) within the Framework of the Smart Growth Operative
Programme 2014-2020. The authors acknowledge the support from The Centro de Microanálisis de Materiales (CMAM)—Universidad Autónoma de Madrid,
for the beam time proposal (demonstration of a grating profile for soft X-rays in diamond via ion lithography) with code IuB-005/21, and its technical staff
for their contribution to the operation of the accelerator. We also acknowledge P. Olivero for very useful comments on the manuscript draft
and Innovation, TechnoFusión (III)-CM (S2018/EMT-4437) from Comunidad de Madrid (cofinanced by ERDF and ESF), agreement between Community
of Madrid and Universidad Autónoma de Madrid (item “Excellence of University Professorate”). M.L.C. acknowledges financial support from the research
project “Captacion de Talento UAM” Ref: #541D300 supervised by the Vice-Chancellor of Research of Universidad Autónoma de Madrid (UAM). LOREA
beamline at ALBA is a project co-funded by the European Regional Development Fund (ERDF) within the Framework of the Smart Growth Operative
Programme 2014-2020. The authors acknowledge the support from The Centro de Microanálisis de Materiales (CMAM)—Universidad Autónoma de Madrid,
for the beam time proposal (demonstration of a grating profile for soft X-rays in diamond via ion lithography) with code IuB-005/21, and its technical staff
for their contribution to the operation of the accelerator. We also acknowledge P. Olivero for very useful comments on the manuscript draft
Antibacterial Films of Silver Nanoparticles Embedded into Carboxymethylcellulose/Chitosan Multilayers on Nanoporous Silicon: A Layer-by-Layer Assembly Approach Comparing Dip and Spin Coating
Digital.CSIC. Repositorio Institucional del CSIC
- Naveas, Nelson
- Pulido, Ruth
- Torres-Costa, Vicente
- Agulló Rueda, F.
- Santibáñez, Mauricio
- Malano, Francisco
- Recio-Sánchez, Gonzalo
- Garrido-Miranda, Karla A.
- Manso-Silván, Miguel
- Hernández-Montelongo, Jacobo
The design and engineering of antibacterial materials are key for preventing bacterial adherence and proliferation in biomedical and household instruments. Silver nanoparticles (AgNPs) and chitosan (CHI) are broad-spectrum antibacterial materials with different properties whose combined application is currently under optimization. This study proposes the formation of antibacterial films with AgNPs embedded in carboxymethylcellulose/chitosan multilayers by the layer-by-layer (LbL) method. The films were deposited onto nanoporous silicon (nPSi), an ideal platform for bioengineering applications due to its biocompatibility, biodegradability, and bioresorbability. We focused on two alternative multilayer deposition processes: cyclic dip coating (CDC) and cyclic spin coating (CSC). The physicochemical properties of the films were the subject of microscopic, microstructural, and surface–interface analyses. The antibacterial activity of each film was investigated against Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive) bacteria strains as model microorganisms. According to the findings, the CDC technique produced multilayer films with higher antibacterial activity for both bacteria compared to the CSC method. Bacteria adhesion inhibition was observed from only three cycles. The developed AgNPs–multilayer composite film offers advantageous antibacterial properties for biomedical applications., his work was financially supported by Fondo Nacional de Desarrollo Científico Tecnológico FONDECYT—Chile (grant number 11180395), CONICYT PFCHA/DOCTORADO/2017-21172001 (Nelson Naveas), PFCHA/DOCTORADO/2015-21151648 (Ruth Pulido), and Vicerrectoría de Investigación y Doctorados de la Universidad San Sebastian—VRIDPuente21/03 project. The work was partially funded by project USAMPSA PID2020-112770RB-C22 from Ministerio de Ciencia e Innovación de España., Peer reviewed
Dataset of Operando Exploration of Tribochemical Decomposition in Synthetic FeS2 thin film and Mineral Iron Pyrite
Digital.CSIC. Repositorio Institucional del CSIC
- Muñoz-Cortés, Esmeralda
- Sánchez-Prieto, Jesús
- Zabala, Borja
- Sánchez, Carlos
- Flores, Eduardo
- Flores, Araceli
- Román García, Elisa Leonor
- Ares, José R.
- Nevshupa, Roman
FeS2 thin films were obtained by sulfuration of Fe coatings, which were deposited by thermal evaporation of iron powder (Goodfellow, 99.99%) on soda lime glass substrates under high vacuum. The initial thickness of the Fe coatings was 300±20 nm as measured using quartz crystal microbalance. The Fe coating was transferred into a glass ampoule, which contained a small amount of sulfur powder (Merck, 99.99%) placed at one end. The ampoule was evacuated down to 10-5 mbar and sealed. Then, sulfur was sublimated by heating to 300ºC for 20 h, while sulfur vapour at a pressure of about 0.065 bar reacted with the Fe film. After sulfuration, the coatings were kept in the same sealed ampoules at room temperature until they were characterized. Natural pyrite was used to contrast the results obtained for artificial FeS2 thin film. A sheet of iron pyrite was cut from a native crystal proceeding from Peru mines and polished. X-ray diffraction analysis showed a typical cubic crystal structure of the mineral sample.
The iron coatings' crystal structure was analyzed both before and after sulfuration using grazing-angle X-ray diffraction (XRD). This was accomplished by employing Cu Kα radiation and maintaining a fixed incidence angle of 1.7°. To determine the mean crystallite size, the Scherrer formalism was applied to the main diffraction band (200). Film thickness measurements were conducted at the film edge utilizing a stylus profilometer, achieving an accuracy of 10 nm.
The mechanical properties of the FeS2 coatings were investigated through nanoindentation (G200, KLA Corp.), utilizing a Berkovich diamond tip in dynamic contact mode. The maximum indentation depth was 100 nm constrained to remain below 10% of the total coating thickness. The loading cycle was carried out at a constant indentation strain rate of 0.1 s-1 and a small oscillating force was superimposed to this loading ramp (75 Hz of frequency, amplitude of 2 nm). Continuous measurement of the contact stiffness was achieved on the basis of the phase lag between the sinusoidal force and the penetration produced.
X-ray Photoemission Spectrometry (XPS) was used to obtain information on chemical state of various elements under ultra-high vacuum (UHV) with a pressure below 10-8 Pa. Mg Kα radiation with an energy of 1253.6 eV was employed. To eliminate any airborne adsorbed contaminants from the sample surface, ensuring a pristine surface for subsequent XPS analysis, the samples underwent Ar+ ion sputtering with an energy of 1 keV and an incident angle of 60° with respect to the sample normal. The sputtering depth was around 1.3 Å. It should be noted that Ar+ ions for sputtering can potentially alter the chemical oxidation state of Fe and/or S and/or change the surface composition due to preferential sputtering. No additional treatment was performed. High-resolution XPS analysis of Fe 2p, S 2p, O 1s, and C 1s was conducted through the fitting process employing the minimum possible number of components compatible with the expected chemistry. For instance, both the Fe 2p3/2 and Fe 2 p1/2 spin-orbit peaks were fitted to ensure the coherence of the procedure, while assuming a Shirley background. For the sake of simplicity, only the Fe 2p3/2 bands are discussed here. The S 2p peak was fitted employing a S 2p3/2 S 2p1/2 doublet, considering the theoretical spin-orbit coupling ratio of 1:2. A fixed separation of 1.2 eV between the S 2p3/2 and S 2p1/2 was maintained based on literature for data processing., Electron Stimulated Desorption (ESD) coupled with mass spectrometry was used to examine the chemical composition of the adsorbed layers and the surface chemical groups. The sample was bombarded with electrons using an electron gun positioned at a 60° angle to the surface normal. Unless otherwise mentioned, the electron energy used was 600 eV. The ions, which were generated on the surface due to electron bombardment, released from the sample and were detected using a quadrupole mass spectrometer, situated in front of the sample. More details about the setup and process of the ESD experimental system can be found elsewhere.
Thermal Gravimetric analysis of thin films was used to analyse the gases emitted during progressive heating under both Ar and dry air flows using a mass spectrometer. The rate of linear heating was set at 5, 10, and 20 °C/min. The emitted gases were analysed in the range of 1-90 a.m.u.
The Rutherford Backscattering Spectrometry (RBS) and Elastic Recoil Detection Analysis (ERDA) techniques, available at the Centre of Microanalysis of Materials of Autonomous University of Madrid, were employed to determine the elemental composition of the sample surfaces. Its 5MV linear tandem accelerator facility provides the ion beams to carry out the characterization with these techniques. In this study, a collimated He+ beam with energies of 3.035 or 4.260 MeV extracted from the accelerator was used, while choice of these energies’ values justified under resonant conditions for oxygen and carbon respectively. For RBS analysis, the backscattered ions were detected at an angle of 170° with respect to the direction of the incident ion beam. In the case of ERDA, the ions were directed to the surface at an incident angle of 75° with respect to the surface normal. Recoiled particles were collected at 30°. To filter out heavier ions, a 19 µm thick mylar film was placed in front of the detector to obtain the hydrogen depth profile. The total ion dose in each measurement was set to 15 µC with a particle flux of 5.5x1012 cm-2 s-1 and a probe size of 1.5x1.5 mm2. The spectra were taken with the samples at random orientations. For energy-to-depth conversion, common SRIM (Stopping and Range of Ions in Matter) energy loss data were used, along with reference samples of MgH2 Er-doped TiO2 coatings. The RBS-ERDA spectra were fitted using SIMNRA simulation software.
The gases emitted during mechanical activation of the materials were analysed using an original UHV experimental system equipped with a quadrupole mass spectrometer (Hiden HALO), a reciprocating motion UHV-grade friction cell, and a dynamic gas expansion system. Such a configuration allows accurate quantification of minute emission rates down to 1 pmol s-1. The samples were rubbed under UHV using alumina spheres, 3 mm in diameter. The rubbing conditions, unless otherwise stated, were as follows: the normal load of 0.44 N, the frequency of reciprocating motion of 1 s-1, and the mean rubbing velocity of 0.18 m s-1. The experimental system is schematically shown in Figure 1 and described in detail elsewhere. Before the tests, the alumina spheres were thoroughly degreased consecutively in acetone and isopropanol ultrasonic baths. After drying, they were submerged in a hot Piranha solution to remove carbon and metal residues, rinsed with ultrapure water, and dried in an N2 stream. The differential mass spectra (DMS) were derived by subtracting the mean steady background mass spectra from the mean mass spectra recorded during the application of the mechanical stimulus. Only statistically significant changes (α=0.05) in DMS were analysed among the channels within the 1 – 100 a.m.u. range. To ensure comparability, the mass spectra were normalized by dividing by the total ion current in each spectrum. The tentative identification of ion species was based on reference cracking patterns from the NIST Webbook (NIST Webbook). The gas composition was determined through a backward stepwise regression method, in which we utilized reference mass spectra of various potential gas precursors. These spectra were fitted in various combinations to the experimental DMS with the aim of identifying the combination that included the fewest precursors and achieved a high R2adj value. Behavioural analysis (BA) was employed to develop better understanding of the mechanisms of underlying tribochemical processes. BA allows to explore the short- and long-term trends of highly dynamic emission time series, to establish the degree of correlation between the mass spectrometer signals, and to trace them back to the possible emission sources in the mechanically affected bulk material and/or on the mechanically affected surfaces.
Chemical changes in the Mechanically Affected Zones (MAZ) were studied using vibrational spectroscopy (Raman and FTIR). All the results were benchmarked against the spectra obtained from neighbouring pristine surfaces. Raman spectra were measured using a 532 nm laser in air. Infrared micro-reflectance spectra were obtained using a micro-FTIR spectrometer., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal tribochemical decomposition of synthetic thin-film iron sulphide and mineral iron pyrite. Tribochemical reactions were studied on a micrometre scale using localized rubbing under ultrahigh vacuum. Mechanically Stimulated Gas Emission Mass-Spectrometry (MSGE-MS) including the Dynamic gas expansion method was used to determine the kinetic parameters of gas emission and the composition of the emitted gases. The study was complemented by structural, morphological, tribological, mechanical and surface analyses. It was found that carbon-containing gases were dominating. The sulfur-containing gases comprised H2S, COS and CS2. The latter two were unexpected. The emission of these gases was traced back to solid-state chemical reactions kinetically controlled by the precursor concentrations and driven through non-thermal mechanisms, which we tentatively assigned to formation of sulfur radicals., This study was co-funded by Spanish Ministry for Science and Innovation (grants PID2019-111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00) and funding from Madrid Community (project S2018/NMT-4291 TEC2SPACE), Ministry of Science and Innovation of Spain (project CSIC13-4E-1794) and EU (FEDER, FSE)., 1. Dataset of mass-spectrometry time series of mechanically stimulated gas emission from sodium alanate (NaAlH4) pellets under vacuum.-- 2. Dataset of Thermal Programmed Desorption – Mass-Spectrometry (TPD-MS) analysis of sodium alanate.-- 3. Dataset of X-ray diffraction of sodium alanate.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of sodium alanate.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of sodium alanate., No
The iron coatings' crystal structure was analyzed both before and after sulfuration using grazing-angle X-ray diffraction (XRD). This was accomplished by employing Cu Kα radiation and maintaining a fixed incidence angle of 1.7°. To determine the mean crystallite size, the Scherrer formalism was applied to the main diffraction band (200). Film thickness measurements were conducted at the film edge utilizing a stylus profilometer, achieving an accuracy of 10 nm.
The mechanical properties of the FeS2 coatings were investigated through nanoindentation (G200, KLA Corp.), utilizing a Berkovich diamond tip in dynamic contact mode. The maximum indentation depth was 100 nm constrained to remain below 10% of the total coating thickness. The loading cycle was carried out at a constant indentation strain rate of 0.1 s-1 and a small oscillating force was superimposed to this loading ramp (75 Hz of frequency, amplitude of 2 nm). Continuous measurement of the contact stiffness was achieved on the basis of the phase lag between the sinusoidal force and the penetration produced.
X-ray Photoemission Spectrometry (XPS) was used to obtain information on chemical state of various elements under ultra-high vacuum (UHV) with a pressure below 10-8 Pa. Mg Kα radiation with an energy of 1253.6 eV was employed. To eliminate any airborne adsorbed contaminants from the sample surface, ensuring a pristine surface for subsequent XPS analysis, the samples underwent Ar+ ion sputtering with an energy of 1 keV and an incident angle of 60° with respect to the sample normal. The sputtering depth was around 1.3 Å. It should be noted that Ar+ ions for sputtering can potentially alter the chemical oxidation state of Fe and/or S and/or change the surface composition due to preferential sputtering. No additional treatment was performed. High-resolution XPS analysis of Fe 2p, S 2p, O 1s, and C 1s was conducted through the fitting process employing the minimum possible number of components compatible with the expected chemistry. For instance, both the Fe 2p3/2 and Fe 2 p1/2 spin-orbit peaks were fitted to ensure the coherence of the procedure, while assuming a Shirley background. For the sake of simplicity, only the Fe 2p3/2 bands are discussed here. The S 2p peak was fitted employing a S 2p3/2 S 2p1/2 doublet, considering the theoretical spin-orbit coupling ratio of 1:2. A fixed separation of 1.2 eV between the S 2p3/2 and S 2p1/2 was maintained based on literature for data processing., Electron Stimulated Desorption (ESD) coupled with mass spectrometry was used to examine the chemical composition of the adsorbed layers and the surface chemical groups. The sample was bombarded with electrons using an electron gun positioned at a 60° angle to the surface normal. Unless otherwise mentioned, the electron energy used was 600 eV. The ions, which were generated on the surface due to electron bombardment, released from the sample and were detected using a quadrupole mass spectrometer, situated in front of the sample. More details about the setup and process of the ESD experimental system can be found elsewhere.
Thermal Gravimetric analysis of thin films was used to analyse the gases emitted during progressive heating under both Ar and dry air flows using a mass spectrometer. The rate of linear heating was set at 5, 10, and 20 °C/min. The emitted gases were analysed in the range of 1-90 a.m.u.
The Rutherford Backscattering Spectrometry (RBS) and Elastic Recoil Detection Analysis (ERDA) techniques, available at the Centre of Microanalysis of Materials of Autonomous University of Madrid, were employed to determine the elemental composition of the sample surfaces. Its 5MV linear tandem accelerator facility provides the ion beams to carry out the characterization with these techniques. In this study, a collimated He+ beam with energies of 3.035 or 4.260 MeV extracted from the accelerator was used, while choice of these energies’ values justified under resonant conditions for oxygen and carbon respectively. For RBS analysis, the backscattered ions were detected at an angle of 170° with respect to the direction of the incident ion beam. In the case of ERDA, the ions were directed to the surface at an incident angle of 75° with respect to the surface normal. Recoiled particles were collected at 30°. To filter out heavier ions, a 19 µm thick mylar film was placed in front of the detector to obtain the hydrogen depth profile. The total ion dose in each measurement was set to 15 µC with a particle flux of 5.5x1012 cm-2 s-1 and a probe size of 1.5x1.5 mm2. The spectra were taken with the samples at random orientations. For energy-to-depth conversion, common SRIM (Stopping and Range of Ions in Matter) energy loss data were used, along with reference samples of MgH2 Er-doped TiO2 coatings. The RBS-ERDA spectra were fitted using SIMNRA simulation software.
The gases emitted during mechanical activation of the materials were analysed using an original UHV experimental system equipped with a quadrupole mass spectrometer (Hiden HALO), a reciprocating motion UHV-grade friction cell, and a dynamic gas expansion system. Such a configuration allows accurate quantification of minute emission rates down to 1 pmol s-1. The samples were rubbed under UHV using alumina spheres, 3 mm in diameter. The rubbing conditions, unless otherwise stated, were as follows: the normal load of 0.44 N, the frequency of reciprocating motion of 1 s-1, and the mean rubbing velocity of 0.18 m s-1. The experimental system is schematically shown in Figure 1 and described in detail elsewhere. Before the tests, the alumina spheres were thoroughly degreased consecutively in acetone and isopropanol ultrasonic baths. After drying, they were submerged in a hot Piranha solution to remove carbon and metal residues, rinsed with ultrapure water, and dried in an N2 stream. The differential mass spectra (DMS) were derived by subtracting the mean steady background mass spectra from the mean mass spectra recorded during the application of the mechanical stimulus. Only statistically significant changes (α=0.05) in DMS were analysed among the channels within the 1 – 100 a.m.u. range. To ensure comparability, the mass spectra were normalized by dividing by the total ion current in each spectrum. The tentative identification of ion species was based on reference cracking patterns from the NIST Webbook (NIST Webbook). The gas composition was determined through a backward stepwise regression method, in which we utilized reference mass spectra of various potential gas precursors. These spectra were fitted in various combinations to the experimental DMS with the aim of identifying the combination that included the fewest precursors and achieved a high R2adj value. Behavioural analysis (BA) was employed to develop better understanding of the mechanisms of underlying tribochemical processes. BA allows to explore the short- and long-term trends of highly dynamic emission time series, to establish the degree of correlation between the mass spectrometer signals, and to trace them back to the possible emission sources in the mechanically affected bulk material and/or on the mechanically affected surfaces.
Chemical changes in the Mechanically Affected Zones (MAZ) were studied using vibrational spectroscopy (Raman and FTIR). All the results were benchmarked against the spectra obtained from neighbouring pristine surfaces. Raman spectra were measured using a 532 nm laser in air. Infrared micro-reflectance spectra were obtained using a micro-FTIR spectrometer., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal tribochemical decomposition of synthetic thin-film iron sulphide and mineral iron pyrite. Tribochemical reactions were studied on a micrometre scale using localized rubbing under ultrahigh vacuum. Mechanically Stimulated Gas Emission Mass-Spectrometry (MSGE-MS) including the Dynamic gas expansion method was used to determine the kinetic parameters of gas emission and the composition of the emitted gases. The study was complemented by structural, morphological, tribological, mechanical and surface analyses. It was found that carbon-containing gases were dominating. The sulfur-containing gases comprised H2S, COS and CS2. The latter two were unexpected. The emission of these gases was traced back to solid-state chemical reactions kinetically controlled by the precursor concentrations and driven through non-thermal mechanisms, which we tentatively assigned to formation of sulfur radicals., This study was co-funded by Spanish Ministry for Science and Innovation (grants PID2019-111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00) and funding from Madrid Community (project S2018/NMT-4291 TEC2SPACE), Ministry of Science and Innovation of Spain (project CSIC13-4E-1794) and EU (FEDER, FSE)., 1. Dataset of mass-spectrometry time series of mechanically stimulated gas emission from sodium alanate (NaAlH4) pellets under vacuum.-- 2. Dataset of Thermal Programmed Desorption – Mass-Spectrometry (TPD-MS) analysis of sodium alanate.-- 3. Dataset of X-ray diffraction of sodium alanate.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of sodium alanate.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of sodium alanate., No
Operando exploration of tribochemical decomposition of FeS2 thin films and mineral iron pyrite
Digital.CSIC. Repositorio Institucional del CSIC
- Muñoz-Cortés, Esmeralda
- Sánchez-Prieto, Jesús
- Zabala, Borja
- Sánchez, Carlos
- Flores, Eduardo
- Flores, Araceli
- Román García, Elisa Leonor
- Ares, José R.
- Nevshupa, Roman
Tribochemical decomposition of thin-film synthetic iron disulfide and mineral iron pyrite was studied using a combination of operando mass-spectrometry coupled to ultrahigh vacuum tribochemical cell and these gas expansion system. The composition and kinetics of gas emission were analyzed using an original methodology. It was found that carbon-containing gases were dominating. The sulfur-containing gases comprised H2S, COS and CS2. The latter two were unexpected. The emission of the gases was traced back to solid-state chemical reactions kinetically controlled by the precursor concentrations and driven through non-thermal mechanisms, which we tentatively assigned to formation of sulfur radicals., This work was supported by the Ministry of Science, Innovation and University of Spain (grants PID2019-
111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00). We acknowledge the service from the MiNa Laboratory at IMN and funding from Madrid Community (project S2018/NMT-4291 TEC2SPACE), Ministry of Science, Innovation and Universities of Spain (project CSIC13-4E-1794), and EU (FEDER, FSE) The authors acknowledge the support from The Centre for Micro Analysis of Materials (CMAM)—Universidad Autónoma de Madrid, for the beam time proposal (Analysis of surface elemental transformations induced by mechanochemical reactions with
metal sulfides) with code STD-022/23, and its technical staff for their contribution to the operation of the accelerator., Peer reviewed
111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00). We acknowledge the service from the MiNa Laboratory at IMN and funding from Madrid Community (project S2018/NMT-4291 TEC2SPACE), Ministry of Science, Innovation and Universities of Spain (project CSIC13-4E-1794), and EU (FEDER, FSE) The authors acknowledge the support from The Centre for Micro Analysis of Materials (CMAM)—Universidad Autónoma de Madrid, for the beam time proposal (Analysis of surface elemental transformations induced by mechanochemical reactions with
metal sulfides) with code STD-022/23, and its technical staff for their contribution to the operation of the accelerator., Peer reviewed
Femtosecond laser thinning for resistivity control of tungsten ditelluride thin-films synthesized from sol-gel deposited tungsten oxide
Digital.CSIC. Repositorio Institucional del CSIC
- Fernández García, A.
- García-Lechuga, Mario
- Agulló Rueda, F.
- Rubio-Zuazo, Juan
- Manso Silvan, M.
8 pags., 7 figs., In this work we present a route for fabricating WTe thin-films together with femtosecond laser post processing, enabling to finely control the conductivity. First, we produce amorphous films of WO on Si by spin-coating a sol-gel precursor followed by a consolidating annealing and a reduction process in partial H atmosphere, leading to porous metallic tungsten cluster layers. To achieve WTe, the films were exposed to the chalcogen vapours by isothermal closed space vapor transport. The formation of a tungsten ditelluride film composed of piled crystals could be confirmed and a gradient of surface rich Te identified through hard X-ray photoelectron spectroscopy. Finally, it is demonstrated that resistivity can be changed from 0.2 mΩ.m to 1 mΩ.m, while keeping the material characteristics. An anisotropic conductivity can be induced by direct selective thinning with fs laser writing (350 fs pulse duration, 515 nm laser wavelength) of 1D stripes. The obtained results, demonstrate that laser processing is a promising thin-film post-processing technique that can be applied to 2D transition metal dichalcogenide thin films., The current research was funded through grants PID2020–112770RB-C21 and PID2020–112770RB-C22 by MCIN/AEI/10.13039/501100011033. We acknowledge the Spanish MCIN and CSIC for provision of synchrotron radiation at the Spanish line at the ESRF trough project 25–02–972. We acknowledge the service from the MiNa Laboratory at IMN, and funding from CM (project S2018/NMT-4291 TEC2SPACE), MINECO (project CSIC13–4E-1794) and EU (FEDER, FSE).
Dataset of Exploring Tribochemical Transduction Pathways for Dehydrogenation of Molecular Hydrides
Digital.CSIC. Repositorio Institucional del CSIC
- Muñoz-Cortés, Esmeralda
- Leardini, Fabrice
- Conte, Marcello
- Campo, Ángel Adolfo del
- Flores, Eduardo
- Ares, José R.
- Nevshupa, Roman
Cylindrical pellets 13 mm in diameter and ca. 2 mm thick were obtained by compacting, under uniaxial pressure of 65 MPa, of commercial powder of EDAB (Boron Specialties, 97% purity). The pellets were prepared and conserved under a static Ar atmosphere before and after the tests. X-ray diffraction (Cu Kα radiation, θ/2θ configuration, 10° - 60° 2θ range) was used to analyze the pellet structure. Thermal gravimetric analysis coupled with mass spectrometry (TGA-MS) under argon flow (heating rate: 10°C/min) was used to evaluate thermal stability and the composition of emitted gases. During the isothermal test the required temperature was attained at a heating rate 10 ºC/min and then maintained constant for 90-380 min depending on the temperature. The ion currents were measured in the range of mass-to-charge ratios from 1 to 90.
Micro-Raman confocal spectrometry (incident laser: 532 nm, power: 5.6 mW) and FTIR microscopy was used to analyze the chemical structure of mechanically affected zones compared to pristine areas. It was conducted under normal atmosphere. In-plane thermal conductivity of EDAB pellets was determined using van der Pauw method.
Nanoindentation with a Berkovich diamond tip (load: 5-20 mN, peak load hold time: 120 s, loading/unloading rates: 4-40 mN/min, 10 measurements for each load) was used to characterize mechanical properties.
Tribochemical reactions under vacuum were studied in real time using Mechanically Stimulated Gas Emission Mass Spectrometry (MSGE-MS) which was described in detail elsewhere. This technique combines a mass-spectrometry, a nearly zero-emission ultrahigh vacuum friction cell and a dynamic gas expansion system. The latter allows for accurate quantification of emitted gas rates with the detection limit around 1 pmol/s. The tribostimulation of the pellets was done using an alumina ball, 3 mm in diameter, under normal load 0.44-1.1 N and the frequency of reciprocating motion 1 full cycle (forward and backward strokes) per second. The additional arrangements which were made to avoid undesirable gas emission sources other than triboemission from mechanically affected zones of the sample are described in ESI. The tribostimulated gas emission was determined from the mass-spectrometry signal and benchmarked against the steady background gas pressure with the indenter standing still. The Differential Mass-Spectra (DMS) were derived by subtracting the reference spectrum from the mass-spectra measured during tribostimulation.
A separate experiment to investigate possible chemical changes in the EDAB under applied mechanical deformation was conducted using Nuclear Magnetic Resonance (NMR). For this experiment about 0.5 g of EDAB powder was grounded in a porcelain mortar just prior to the NMR analysis. A portion of the ground EDAB was analyzed using solid state Magic Angle Spinning (MAS) 1H and 11B NMR, while the other one was analyzed using 1H and 11B solution RMN using deuterated dimethyl sulfoxide (DMSO-d6) as a solvent., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal dehydrogenation of ethane 1,2-diamineborane through the application of mechanical energy. This study investigates whether the tribochemical approach can also be effective to release hydrogen from molecular hydrides such as ethane 1,2-diamineborane (EDAB). Surprisingly, despite dehydrogenating at a lower temperature than metal and complex hydrides, EDAB exhibited faint hydrogen release under mechanical stress. To understand this behavior, the tribochemical decomposition pathways of EDAB were investigated using operando Mechanically Stimulated Gas Emission Mass Spectrometry in combination with other surface and material characterization techniques. The lack of hydrogen emission from EDAB is attributed to a combination of strong intramolecular bonds (covalent and dative bonds) within the molecule, and weak intermolecular interactions (hydrogen bonds and van der Waals forces) between EDAB molecules., This study was co-funded by the Ministry of Science and Innovation of Spain (grants PID2019-111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00)., 1.Dataset of mass-spectrometry time series of mechanically stimulated gas emission from ethane 1,2 dimineborane pellets under vacuum.-- 2. Dataset of Thermal Gravimetry – Mass-Spectrometry (TGA-MS) analysis of ethane 1,2 diamineborane.-- 3. Dataset of X-ray diffraction of ethane 1,2-diamineborane.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of ethane 1,2-diamineborane.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of ethane 1,2-diamineborane.-- 6. Dataset of microindentation of pellets of ethane 1,2-diamineborane.-- 7. Dataset of friction force time-series measured during reciprocating rubbing of pellets of ethane 1,2-diamineborane under vacuum.-- 8. Dataset of Nuclear Magnetic Resonance (RMN EDAB) solid and liquid., No
Micro-Raman confocal spectrometry (incident laser: 532 nm, power: 5.6 mW) and FTIR microscopy was used to analyze the chemical structure of mechanically affected zones compared to pristine areas. It was conducted under normal atmosphere. In-plane thermal conductivity of EDAB pellets was determined using van der Pauw method.
Nanoindentation with a Berkovich diamond tip (load: 5-20 mN, peak load hold time: 120 s, loading/unloading rates: 4-40 mN/min, 10 measurements for each load) was used to characterize mechanical properties.
Tribochemical reactions under vacuum were studied in real time using Mechanically Stimulated Gas Emission Mass Spectrometry (MSGE-MS) which was described in detail elsewhere. This technique combines a mass-spectrometry, a nearly zero-emission ultrahigh vacuum friction cell and a dynamic gas expansion system. The latter allows for accurate quantification of emitted gas rates with the detection limit around 1 pmol/s. The tribostimulation of the pellets was done using an alumina ball, 3 mm in diameter, under normal load 0.44-1.1 N and the frequency of reciprocating motion 1 full cycle (forward and backward strokes) per second. The additional arrangements which were made to avoid undesirable gas emission sources other than triboemission from mechanically affected zones of the sample are described in ESI. The tribostimulated gas emission was determined from the mass-spectrometry signal and benchmarked against the steady background gas pressure with the indenter standing still. The Differential Mass-Spectra (DMS) were derived by subtracting the reference spectrum from the mass-spectra measured during tribostimulation.
A separate experiment to investigate possible chemical changes in the EDAB under applied mechanical deformation was conducted using Nuclear Magnetic Resonance (NMR). For this experiment about 0.5 g of EDAB powder was grounded in a porcelain mortar just prior to the NMR analysis. A portion of the ground EDAB was analyzed using solid state Magic Angle Spinning (MAS) 1H and 11B NMR, while the other one was analyzed using 1H and 11B solution RMN using deuterated dimethyl sulfoxide (DMSO-d6) as a solvent., Datasets of mass-spectrometry signals were obtained in the experiments with non-thermal dehydrogenation of ethane 1,2-diamineborane through the application of mechanical energy. This study investigates whether the tribochemical approach can also be effective to release hydrogen from molecular hydrides such as ethane 1,2-diamineborane (EDAB). Surprisingly, despite dehydrogenating at a lower temperature than metal and complex hydrides, EDAB exhibited faint hydrogen release under mechanical stress. To understand this behavior, the tribochemical decomposition pathways of EDAB were investigated using operando Mechanically Stimulated Gas Emission Mass Spectrometry in combination with other surface and material characterization techniques. The lack of hydrogen emission from EDAB is attributed to a combination of strong intramolecular bonds (covalent and dative bonds) within the molecule, and weak intermolecular interactions (hydrogen bonds and van der Waals forces) between EDAB molecules., This study was co-funded by the Ministry of Science and Innovation of Spain (grants PID2019-111063RB-I00, PID2020-112770RB-C22, PID2020-117573GB-I00, RTI2018-099794-B-I00, and TED2021-129950B-I00)., 1.Dataset of mass-spectrometry time series of mechanically stimulated gas emission from ethane 1,2 dimineborane pellets under vacuum.-- 2. Dataset of Thermal Gravimetry – Mass-Spectrometry (TGA-MS) analysis of ethane 1,2 diamineborane.-- 3. Dataset of X-ray diffraction of ethane 1,2-diamineborane.-- 4. Dataset of micro-FTIR spectra of pristine and mechanically activated surfaces of pellets of ethane 1,2-diamineborane.-- 5. Dataset of Raman spectra measured on the surfaces of pellets of ethane 1,2-diamineborane.-- 6. Dataset of microindentation of pellets of ethane 1,2-diamineborane.-- 7. Dataset of friction force time-series measured during reciprocating rubbing of pellets of ethane 1,2-diamineborane under vacuum.-- 8. Dataset of Nuclear Magnetic Resonance (RMN EDAB) solid and liquid., No
Out-of-plane preferential growth of 2D molybdenum diselenide nanosheets on laser-induced periodic surface structures
Digital.CSIC. Repositorio Institucional del CSIC
- Fernández García, A.
- Ariza, Rocío
- Solís Céspedes, Javier
- Agulló Rueda, F.
- Manso Silvan, M.
- García-Lechuga, Mario
7 pags., 5 figs., In this study, we explore the morphology and orientation of molybdenum diselenide, a Van der Waals 2D material, through isothermal closed space vapor deposition on both pristine and laser-structured substrates. Laser structuring is conducted on dielectric (sapphire), semiconductor (silicon), and conductive (titanium nitride) substrates using ultrashort laser pulses, resulting in smooth topographic changes such as laser-induced periodic surface structures (LIPSS) or selective ablation. Scanning electron microscopy (SEM) reveals the pivotal role of surface structuring in the growth of out-of-plane MoSe nanosheets. This effect is particularly pronounced on monocrystalline substrates like sapphire and silicon, exhibiting in-plane growth on pristine substrates. Additionally, Raman spectroscopy confirms the vertical orientation of flakes on structured substrates and highlights the presence of active edge sites by demonstrating an increased abundance of deposited material. Overall, our findings emphasize the controllability of directing the growth of MoSe flakes through appropriate pre-treatment of the substrate, with potential applications in various fields, including Surface-Enhanced Raman Scattering (SERS). Furthermore, the scalability, reproducibility, and applicability to any substrate make ultrashort laser structuration a promising general strategy for orienting 2D materials., The current research was funded through grants PID2020-112770RB-C21 and PID2020-112770RB-C22 funded by MCIN/AEI/10.13039/501100011033. We acknowledge the service from the MiNa Laboratory at IMN, and funding from CM (project S2018/NMT-4291 TEC2SPACE), MINECO (project CSIC13-4E-1794) and EU (FEDER, FSE). The initial part of the research leading to these results has received funding from LASERLAB-EUROPE (grant agreement no. 871124, European Union’s Horizon 2020 research and innovation programme. Grant project CNRS‐LP3002707).
Optoplasmonic tuneable response by femtosecond laser irradiation of glass with deep-implanted gold nanoparticles
Digital.CSIC. Repositorio Institucional del CSIC
- Solana-Ramírez, Irene
- Ynsa, María Dolores
- Cabello, Fátima
- Chacón, Fernando
- Siegel, Jan
- García-Lechuga, Mario
8 pages, 5 figures, The manipulation of the optical properties of plasmonic nanocomposites is of high interest for the development of advanced optical devices with tailored unique properties. Achieving these objectives requires a combination of synthesis techniques and post-fabrication strategies. Here, we combine the use of two well-established physical strategies: MeV ion implantation and femtosecond laser processing. Firstly, we synthesize Au-doped soda lime glass nanocomposite through ion beam implantation (Au2+ at 1.8 MeV) followed by thermal annealing. This synthesis procedure results in a peculiar optical response based on the combination of Au-nanoparticle plasmonic resonance and a Fabry-Perot interference, caused by the deep implantation (centered at 480 nm). Secondly, this dual response is demonstrated to be highly tuneable by non-resonant femtosecond laser irradiation (800-nm wavelength and 130-fs pulse duration). Depending on the laser fluence, three transformation regimes are distinguished: supressing the interferometric response by spallative ablation, inducing vivid blue colors by surface swelling, and producing red-shifted color changes by multi-shot irradiation at low fluences. The proposed method is very versatile, since it is applicable to any dielectric matrix or implanted element. This work paves the way to a new route for the development of scalable and tuneable nanocomposites with several potential applications in optics., The current research was funded through grants ULS_PSB(PID2020112770RB-C21 and PID2020-112770RB-C22) funded by MCIN/AEI/ 10.13039/501100011033 and ASSESS (TED2021-129666B-C22) funded by MCIN/AEI/10.13039/501100011033 and the European Union NextGenerationEU/PRTR. Authors acknowledge the support from CMAM-UAM for the beam time (STD045/22, STD009/23, STD024/23 and STD025/23) and its technical staff support, in particular to Jesús S´anchez Prieto. Authors acknowledge the use of instrumentation as well as the technical advice provided by the National Facility ELECMI ICTS, node "Laboratorio de Microscopías Avanzadas" at the University of Zaragoza. I. S. acknowledges for their support and help in RBS analysis to Jose Gonzalo de los Reyes (IO, CSIC) and Gaston García Lopez (CMAM-UAM)., Peer reviewed
DOI: http://hdl.handle.net/10261/374611, https://api.elsevier.com/content/abstract/scopus_id/85206258472
Iodine-substituted hydroxyapatite nanoparticles and activation of derived ceramics for range verification in proton therapy
UPCommons. Portal del coneixement obert de la UPC
- Magro Hernández, Raúl
- Muñoz Noval, Alvaro
- Briz, José Antonio
- Rodríguez Murias, Javier
- Espinosa Rodríguez, Andrea
- Fraile, Luis Mario
- Agulló Rueda, Fernando
- Ynsa, Maria Dolores
- Tavares de Sousa, Célia
- Cortés Llanos, Belén
- García López, Gastón
- Nacher González, Enrique
- García Távora, Vicente
- Mont i Geli, Nil|||0000-0003-4249-7281
- Nerio Aguirre, Amanda
- Valladolid Onecha, Víctor
- Pallàs i Solís, Max|||0000-0001-6137-0812
- Tarifeño Saldivia, Ariel
- Tengblad, Olof Erik
- Manso Silvan, Miguel
- Viñals Onsens, Silvia
Osteosarcoma is a radioresistant cancer, and proton therapy is a promising radiation alternative for treating cancer with the advantage of a high dose concentration in the tumor area. In this work, we propose the use of iodine-substituted hydroxyapatite (IHAP) nanomaterials to use iodine (127I) as a proton radiation tracer, providing access to range verification studies in mineralized tissues. For this purpose, the nanomaterials were synthesized at four iodine concentrations via hydrothermal synthesis. The materials were characterized via different microstructural techniques to identify an optimal high iodine concentration and pure apatite phase nanomaterial. Finally, such pure IHAP powders were shaped and irradiated with proton beams of 6 and 10 MeV, and their activation was demonstrated through subsequent decay analysis. The materials could be integrated into phantom structures for the verification of doses and ranges of protons prior to animal testing and clinical proton therapy treatments of tumors located deep under combined soft and calcified tissues., The current research was funded through grants PID2020-112770RB-C21, PDC2022-133382-I00 and PID2020-112770RB-C22 and PID2023-151371OB-C22 by MCIN/AEI/10.13039/501100011033 and FEDER, EU, grant FLASHOnChip (PLEC2022-009256) by MCIN, ASAP-CM (P2022/BMD-7434) from DGI-Comunidad de Madrid and CIPROM/2021/064 from Generalitat Valenciana. Beamtime at the CMAM through experiment EUB004/22 is acknowledged., Peer Reviewed
Supplementary material for the paper "Process design for the manufacturing of soft X-ray gratings in single-crystal diamond by high-energy heavy-ion irradiation"
e-cienciaDatos, Repositorio de Datos del Consorcio Madroño
- García López, Gastón
- Martin, Maxime
- Ynsa, María Dolores
- Torres-Costa, Vicente
- Olivares, José
- Tardío, Miguel
- Crespillo, Miguel L.
- Bosia, Federico
- Peña-Rodríguez, Ovídio
- Nicolás, Josep
- Tallarida, Massimo
A novel manufacturing process for optical gratings suitable for use in the UV and soft X-ray regimes in a single-crystal diamond substrate based on highly focused swift heavy-ion irradiation. This type of grating is extensively used in light source facilities such as synchrotrons or free electron lasers, with ever-increasing demands in terms of thermal loads, depending on beamline operational parameters and architecture. The process may be a future alternative to current manufacturing techniques, providing the advantage of being applicable to single-crystal diamond substrates, with their unique properties in terms of heat conductivity and radiation hardness.
AFM measured topography of single-crystal diamond sample irradiated with 9 MeV C ions with a dose pattern tuned to obtain a blazed soft X-ray grating.
AFM measured topography of single-crystal diamond sample irradiated with 9 MeV C ions with a dose pattern tuned to obtain a blazed soft X-ray grating.