Dataset.
SERS activity of silver-based calcium silicate hydrate upon laser irradiation
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/371208
Digital.CSIC. Repositorio Institucional del CSIC
- Maestro-Guijarro, Laura
- Martínez-Ramírez, S.
- Sánchez-Cortés, Santiago
- Marco, J.F.
- de la Figuera, Juan
- Castillejo, Marta
- Oujja, Mohamed
- Carmona-Quiroga, Paula
C-S-H and C-S-Ag-H gel solutions were analysed by UV/Vis/NIR spectroscopy with a Shimadzu 3600 UV/Vis/NIR spectrometer equipped with 2H and Wlamps, a photomultiplier (UV/Vis), and a InGaAs and a PbS (NIR) detectors. The baseline reference sample was prepared with 1000 µL of MilliQ water. The samples were diluted 1:19 (50 μL of gel solution to 950 μL of of MilliQ water) and the measurements were recorded in the range of 190–850 nm, with slow scan speed. The sampling interval and the slit width were 0.5 nm and 1 nm, respectively. For the 29Si NMR analysis of dried C-S-H and C-S-Ag-H, a Bruker AV-400 (9.4 T and νR of 4 kHz) (Bruker, Germany) NMR spectrometer was used in the following conditions: pulse width of 7 μs and relaxation delay of 60 s with typically 3000 scans. The 29Si chemical shifts were determined relative to tetramethylsilane. The spectra were treated for band deconvolution into Gaussian peaks and fitted using Origin 2022 software.
The micro-Raman spectra were carried out on pressed pellets of the samples with a Raman microscope Renishaw RM1000 (Renishaw, Wotton-under-Endge, UK) equipped with a Leica microscope and an electrically refrigerated CCD camera. Laser excitation line was provided by a He:Ne (633 nm wavelength, 25 mW output power with approximately 2 mW at the sample). The spectra were obtained using a 50× magnification objective, a spectral resolution of 4 cm−1, a 10 s exposure time, 5 accumulations, and 2mW laser power per spectra in the range of 2000–100 cm−1 in order to increase signal/noise ratio. The frequencies were calibrated with silicon at 520 cm−1.
X-ray photoelectron (XP) and SERS spectra were taken on pressed C-S-Ag-H pellets before and after irradiation at 355 nm, and 532 nm (and of the reference C-S-H pellet).
For the former technique, the analysis was performed under a base pressure lower than 7.5 · 10−9 Torr using a PHOIBOS-150 (Specs) electron analyzer, Mg Kα radiation and a constant pass energy of 100 eV and 20 eV for the wide and narrow scans, respectively. The pellets were fixed to the sample holder using double-sided conductive carbon tape to ensure a good conductivity and the X-ray gun was used at 100 W power in order to avoid any possible sample degradation induced by the X-ray irradiation. The binding energy scale was referenced to the main C 1s signal of the adventitious carbon contamination layer which was set at 284.8 eV. All the spectra were fitted using pseudo-Voigt lines (30 % Gaussian/70 % Lorentzian) and a Shirley-type background.
For the SERS analysis, the same experimental conditions were used as for obtaining the Raman spectra using Rhodamine B as a probe molecule (an aliquot of 2 µl of a 5 × 10−6 M aqueous solution was dropped on the irradiated and on the non-irradiated silver-containing pellets). Additionally, different reference RhB spectra were acquired on hydroxylamine-reduced silver nanoparticles (NPs), 2 µl dropped on top of both C-S-H and C-S-Ag-H pellets for the comparison of the SERS activities.
More details about samples preparation and irradiation conditions are available in Materials folder., Data life: 2024- (unlimited validity), his is the experimental dataset used in the paper Applied Surface Science, 662: 160107 (2024) (https://doi.org/10.1016/j.apsusc.2024.160107) in which a novel Surface-Enhanced Raman Spectroscopy (SERS) sensor based on a nanostructured substrate, calcium silicate hydrate (C-S-H), the main hydration product of Portland cement, was synthetized. The procedure involves first the incorporation of silver within the nanostructure of the gel (C-S-Ag-H) and second the modification of the surface of pellets of the newly synthesized material by laser irradiation at 532 nm or 355 nm.
This data set includes the results of the effect of silver on the gel structure via visible UV spectroscopy, micro-Raman and
29Si Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR).
It also includes the characterization analyses of the C-S-Ag-H pellets by X-ray Photoelectron Spectroscopy (XPS) to determine the silver oxidation state and the assessment of their SERS activity before and after laser irradiation using for the latter Rhodamine B (RhB) as a probe., We acknowledge financial support from the Spanish State Research Agency (AEI) through projects PID2019-104124RB-I00/AEI/10.13039/501100011033; PID2020-113900RB-I00/AEI/10.13039/ 501100011033; and PID2022-137017OB-I00/AEI/10.13039/501100011033; from European Union’s Horizon 2020 through IPERION HS (Integrated Platform for the European Research Infrastructure ON Heritage Science, GA 871034) project; and from the Community of Madrid through Maestro-Guijarro’s Youth Guarantee contract (CAM20_IQFR_AI_06)., Materials folder: “Sample_synthesis”; “Laser_irradiation_conditions”
NMR folder: "NMR_readme"; "NMR_C-S-H"; "NMR_C-S-Ag-H"
Raman folder: “Raman_readme"; "Raman_C-S-H"; "Raman_C-S-Ag-H"; "Raman_C-S-H_RhB"; "Raman_C-S-Ag-H_RhB"
SERS folder: "SERS_readme"; "SERS_RhB_C-S-Ag-H_355"; "SERS_RhB_C-S-Ag-H_355_NPs"; "SERS_RhB_C-S-Ag-H_532"; "SERS_RhB_C-S-Ag-H_532_NPs"; "SERS_RhB_C-S-Ag-H_NPs"; "SERS_RhB_C-S-H_NPs"
XPS folder: "XPS_readme"; "XPS_AgAuger_C-S-Ag-H_532"; "XPS_AgAuger_C-S-Ag-H_355"; "XPS_Ag3d_C-S-Ag-H_532"; "XPS_Ag3d_C-S-Ag-H_355"; "XPS_Ag3d_C-S-Ag-H"; "XPS_Ag3d_C-S-H"; "XPS_Ca2p_C-S-Ag-H_532"; "XPS_C1s_C-S-Ag-H_532"; "XPS_wide_C-S-Ag-H_532"; "XPS_wide_C-S-Ag-H_355"; "XPS_wide_C-S-Ag-H"; "XPS_wide_C-S-H"
UV-Vis folder: "UV-VIS_readme"; "UV-VIS_C-S-H"; "UV-VIS_C-S-Ag-H", Peer reviewed
DOI: http://hdl.handle.net/10261/371208, https://doi.org/10.20350/digitalCSIC/16639
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/371208
HANDLE: http://hdl.handle.net/10261/371208, https://doi.org/10.20350/digitalCSIC/16639
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/371208
Ver en: http://hdl.handle.net/10261/371208, https://doi.org/10.20350/digitalCSIC/16639
Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/371208
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Digital.CSIC. Repositorio Institucional del CSIC
oai:digital.csic.es:10261/371208
Dataset. 2024
SERS ACTIVITY OF SILVER-BASED CALCIUM SILICATE HYDRATE UPON LASER IRRADIATION
Digital.CSIC. Repositorio Institucional del CSIC
- Maestro-Guijarro, Laura
- Martínez-Ramírez, S.
- Sánchez-Cortés, Santiago
- Marco, J.F.
- de la Figuera, Juan
- Castillejo, Marta
- Oujja, Mohamed
- Carmona-Quiroga, Paula
C-S-H and C-S-Ag-H gel solutions were analysed by UV/Vis/NIR spectroscopy with a Shimadzu 3600 UV/Vis/NIR spectrometer equipped with 2H and Wlamps, a photomultiplier (UV/Vis), and a InGaAs and a PbS (NIR) detectors. The baseline reference sample was prepared with 1000 µL of MilliQ water. The samples were diluted 1:19 (50 μL of gel solution to 950 μL of of MilliQ water) and the measurements were recorded in the range of 190–850 nm, with slow scan speed. The sampling interval and the slit width were 0.5 nm and 1 nm, respectively. For the 29Si NMR analysis of dried C-S-H and C-S-Ag-H, a Bruker AV-400 (9.4 T and νR of 4 kHz) (Bruker, Germany) NMR spectrometer was used in the following conditions: pulse width of 7 μs and relaxation delay of 60 s with typically 3000 scans. The 29Si chemical shifts were determined relative to tetramethylsilane. The spectra were treated for band deconvolution into Gaussian peaks and fitted using Origin 2022 software.
The micro-Raman spectra were carried out on pressed pellets of the samples with a Raman microscope Renishaw RM1000 (Renishaw, Wotton-under-Endge, UK) equipped with a Leica microscope and an electrically refrigerated CCD camera. Laser excitation line was provided by a He:Ne (633 nm wavelength, 25 mW output power with approximately 2 mW at the sample). The spectra were obtained using a 50× magnification objective, a spectral resolution of 4 cm−1, a 10 s exposure time, 5 accumulations, and 2mW laser power per spectra in the range of 2000–100 cm−1 in order to increase signal/noise ratio. The frequencies were calibrated with silicon at 520 cm−1.
X-ray photoelectron (XP) and SERS spectra were taken on pressed C-S-Ag-H pellets before and after irradiation at 355 nm, and 532 nm (and of the reference C-S-H pellet).
For the former technique, the analysis was performed under a base pressure lower than 7.5 · 10−9 Torr using a PHOIBOS-150 (Specs) electron analyzer, Mg Kα radiation and a constant pass energy of 100 eV and 20 eV for the wide and narrow scans, respectively. The pellets were fixed to the sample holder using double-sided conductive carbon tape to ensure a good conductivity and the X-ray gun was used at 100 W power in order to avoid any possible sample degradation induced by the X-ray irradiation. The binding energy scale was referenced to the main C 1s signal of the adventitious carbon contamination layer which was set at 284.8 eV. All the spectra were fitted using pseudo-Voigt lines (30 % Gaussian/70 % Lorentzian) and a Shirley-type background.
For the SERS analysis, the same experimental conditions were used as for obtaining the Raman spectra using Rhodamine B as a probe molecule (an aliquot of 2 µl of a 5 × 10−6 M aqueous solution was dropped on the irradiated and on the non-irradiated silver-containing pellets). Additionally, different reference RhB spectra were acquired on hydroxylamine-reduced silver nanoparticles (NPs), 2 µl dropped on top of both C-S-H and C-S-Ag-H pellets for the comparison of the SERS activities.
More details about samples preparation and irradiation conditions are available in Materials folder., Data life: 2024- (unlimited validity), his is the experimental dataset used in the paper Applied Surface Science, 662: 160107 (2024) (https://doi.org/10.1016/j.apsusc.2024.160107) in which a novel Surface-Enhanced Raman Spectroscopy (SERS) sensor based on a nanostructured substrate, calcium silicate hydrate (C-S-H), the main hydration product of Portland cement, was synthetized. The procedure involves first the incorporation of silver within the nanostructure of the gel (C-S-Ag-H) and second the modification of the surface of pellets of the newly synthesized material by laser irradiation at 532 nm or 355 nm.
This data set includes the results of the effect of silver on the gel structure via visible UV spectroscopy, micro-Raman and
29Si Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR).
It also includes the characterization analyses of the C-S-Ag-H pellets by X-ray Photoelectron Spectroscopy (XPS) to determine the silver oxidation state and the assessment of their SERS activity before and after laser irradiation using for the latter Rhodamine B (RhB) as a probe., We acknowledge financial support from the Spanish State Research Agency (AEI) through projects PID2019-104124RB-I00/AEI/10.13039/501100011033; PID2020-113900RB-I00/AEI/10.13039/ 501100011033; and PID2022-137017OB-I00/AEI/10.13039/501100011033; from European Union’s Horizon 2020 through IPERION HS (Integrated Platform for the European Research Infrastructure ON Heritage Science, GA 871034) project; and from the Community of Madrid through Maestro-Guijarro’s Youth Guarantee contract (CAM20_IQFR_AI_06)., Materials folder: “Sample_synthesis”; “Laser_irradiation_conditions”
NMR folder: "NMR_readme"; "NMR_C-S-H"; "NMR_C-S-Ag-H"
Raman folder: “Raman_readme"; "Raman_C-S-H"; "Raman_C-S-Ag-H"; "Raman_C-S-H_RhB"; "Raman_C-S-Ag-H_RhB"
SERS folder: "SERS_readme"; "SERS_RhB_C-S-Ag-H_355"; "SERS_RhB_C-S-Ag-H_355_NPs"; "SERS_RhB_C-S-Ag-H_532"; "SERS_RhB_C-S-Ag-H_532_NPs"; "SERS_RhB_C-S-Ag-H_NPs"; "SERS_RhB_C-S-H_NPs"
XPS folder: "XPS_readme"; "XPS_AgAuger_C-S-Ag-H_532"; "XPS_AgAuger_C-S-Ag-H_355"; "XPS_Ag3d_C-S-Ag-H_532"; "XPS_Ag3d_C-S-Ag-H_355"; "XPS_Ag3d_C-S-Ag-H"; "XPS_Ag3d_C-S-H"; "XPS_Ca2p_C-S-Ag-H_532"; "XPS_C1s_C-S-Ag-H_532"; "XPS_wide_C-S-Ag-H_532"; "XPS_wide_C-S-Ag-H_355"; "XPS_wide_C-S-Ag-H"; "XPS_wide_C-S-H"
UV-Vis folder: "UV-VIS_readme"; "UV-VIS_C-S-H"; "UV-VIS_C-S-Ag-H", Peer reviewed
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