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Research Services

Servicio de Espectroscopías

Micro-Raman Spectroscopy




Scientific Responsibles
Dr. Juan Carlos Sánchez López, Dr. Hernán Míguez García, Dr. Miguel Angel Centeno Gallego

Technical Assistant
Dr. Miguel Angel Avilés Escaño


Raman spectroscopy is based on a photonic process in which the incident radiation is dis-persed by the sample. This latter is perturbed leading to vibrational and rotational transitions. In general, the Raman spectrum is interpreted like a vibrational one, providing information very similar to the infrared spectroscopy, although the Raman active vibrations are not always the same as those excited with infrared radiation. A Raman vibration mode is active if there is a change of polarizability of the chemical bonds or the considered molecule, which in turn results in the generation of induced dipolar momentam. Its application fields are very broad: semiconductors, carbon compounds (graphite, diamond, nanotubes, fibers…), catalysts, pigments, etc.

Available Equipment

  • LabRAM Horiba Jobin Yvon equipped with a confocal microscope and 3 excitation lasers (785 cm-1 red, 532 cm-1 green, and 325 cm-1 UV)

Contact
jcslopez@icmse.csic.es , h.miguez@csic.es, centeno@icmse.csic.es
954 48 95 43 - 954 48 95 81 - 954 48 95 76



Infrared Spectroscopies




Scientific Responsibles
Dr. Juan Carlos Sánchez López, Dr. Hernán Míguez García, Dr. Miguel Angel Centeno Gallego

Technical Assistant
Dr. Miguel Angel Avilés Escaño


Infrared spectroscopy (FT-IR) is based on the selective absorption of the infrared radiation by the materials. This absorption means a change in the vibrational energy of the chemical bonds, whenever it occurs a change in the polarization. The result is a spectrum showing the absorbed or transmitted radiation as a function of the wavenumber of the radiation, which can be assigned to the corresponding chemical bound.

The equipment at the ICMS works in a wavenumber range from 5000 to 250 cm-1 (CsI optic), and can operate with a gas purge or in vacuum. It is equipped with several accessories to do Diffuse Reflectance (DRIFT), Attenuated Total Reflectance (ATR) or Specular Reflectance. It has got an Infrared Microscope with a lateral resolution of 10 µm.

Available Equipment

  • JASCO FT/IR-6200 IRT-5000

Contact
jcslopez@icmse.csic.es , h.miguez@csic.es, centeno@icmse.csic.es
954 48 95 39



Ultraviolet-Visible Spectroscopies




Scientific Responsibles
Dr. Juan Carlos Sánchez López, Dr. Hernán Míguez García, Dr. Miguel Angel Centeno Gallego

Technical Assistant
Dr. Miguel Angel Avilés Escaño


The Ultraviolet-Visible Spectroscopy (UV-Vis) reports on the existing energy differences be-tween the more external occupied electronic levels and the nearer unoccupied ones.

There are two equipments in the laboratory, which work in the wavelength range of 190 nm to 900 nm. It can operate in the Transmission mode or in Diffuse Reflectance Modes.

Available Equipment

  • Cary 5000+UMA (Universal Measurement Accessory)
  • Cary 300
  • SHIMADZU UV-2101 PC
  • ​Perkin Elmer Lambda 12

Contact
jcslopez@icmse.csic.es , h.miguez@csic.es, centeno@icmse.csic.es
954 48 95 39



Atomic Emission Spectroscopy (ICP-OES)




Scientific Responsibles
Dr. Francisco José Gotor Martínez

Technical Assistant
Lda. Belinda Sigüenza Carballo


Inductively coupled plasma atomic emission spectroscopy (ICP-OES) is an analytical technique that allows the quantification of elements up to the trace level in samples in solution. The sample to be analyzed is nebulized and conducted to an argon plasma, where desolvation, vaporization, atomization and ionization of the elements take place. The atoms and ions reach an excited state by the high thermal energy supplied by the plasma and during the relaxation process electromagnetic radiation is emitted with wavelengths characteristic of each element. The intensity of the different emission lines is proportional to the concentration of the elements, which can be quantified by using appropriate calibration curves. This technique has high detection limits (in the ppb range, μg / L), good reliability, high throughput and multi-elemental capacity, although in some cases spectral interferences can occur due to a high number of emission lines.

Instrumental disponible

  • iCAP 7200 ICP-OES Duo (ThermoFisher Scientific)

Contact
fgotor@cica.es
954 48 95 40


File Formulario ICP.docx

Servicio de Análisis Textural y Térmico

Physisorption-Chemisorption




Scientific Responsibles
Dr. Gerardo Colón Ibáñez, Dr. Miguel Angel Centeno Gallego

Technical Assistant
Dª Cristina Gallardo López


This service constitutes a basic tool for the microstructural characterization of powdered solids of different natures, regarding to their porosity, specific surface area and chemically active surface.

This service is composed by a phyisisorption analyser (Micromeritics, ASAP 2020) which pro-vides the complete adsorption/desorption isotherms, from which the specific surface area, pore and micropore size distribution and concentration of reactive sites are obtained. The instrument is also equipped for carrying out chemisorption of different reactive molecules, as O2, H2, CO, etc.
 

Available Equipment

  • Analizador científico de fisisorción ASAP2010 (Micromeritics)
  • Analizador de quimisorción ASAP2010 (Micromeritics)
  • Analizador de fisisorción multimuestra TRISTAR II (Micromeritics)
  • Analizador de fisisorción multimuestra TRISTAR II-Kr (Micromeritics)

Contact
gcolon@icmse.csic.es, centeno@icmse.csic.es
954 48 95 36 - 954 48 95 43



Thermal Analysis




Scientific Responsibles
Dr. Luis A. Pérez Maqueda

Technical Assistant
Dª Cristina Gallardo López


Thermal analysis techniques allow to studying physical or chemical changes occurring in solid in samples as a function of the temperature. Those changes should involve either a mass change or a heat flow.

The experiments can be performed in the range from room temperature to 1500ºC, both under inert (N2), or reactive (air, O2,…) atmospheres.

Two different techniques are available: Thermogravimetry (TG) and Differential Thermal Analysis (DTA).

Available Equipment

  • TA Instruments Q600 Simultaneous TG/DTA/DSC instrument
  • Thermogravimetric instrument TG, TA Instruments Q5000

Contact
maqueda@cica.es
954 48 95 48



Particle size and Z potential analysis




Scientific Responsibles
Dr. Manuel Ocaña Jurado

Technical Assistant
Dª Cristina Gallardo López


Dynamic light scattering (DLS) and Laser diffraction (LD) are available for the determination of particle size distributions of colloidal systems (dispersed in aqueous or organic dispersions solutions) in the range 3-3000 nanometers (DLS) and 0.05-900 microns (LD).

Electrophoretic mobility measurements can be also performed for the evaluation of Z potential in colloidal systems (aqueous or organic dispersions).
 

Available Equipment

  • Malvern model Zetamaster (DLS) and MalvernSizer (LD)

Contact
mjurado@icmse.csic.es
954 48 95 33



Servicio de Microscopía de Electrones

Scanning Electron Microscopy




Scientific Responsibles
Dr. Asunción Fernández Camacho

Technical Assistant
Dra. Mª Carmen Jiménez de Haro


The scanning electron microscopy provides information about the microstructure, morphology and chemical composition at the microscopic scale of solid samples. It can be applied to all type of materials including ceramics, polymers, metals, minerals, catalysts, samples from cultural heritage, thin films, coatings, interfaces, nanoparticles, etc. The SEM microscope is a field emission cold cathode equipment which enables images of the surface morphology and texture of samples with a resolution of 1 nm at 15kV. It also allows working at low voltages with non-metalized samples and in transmission mode for electron-transparent samples (STEM-in-SEM). Coupled to the X-ray detector (EDX) enables compositional analysis and elemental mapping.

Available Equipment

  • Hitachi S4800 SEM-FEG microscope:  cold cathode field emission gun with voltage from 0.5 to 30 kV, resolution of 1nm at 15 kV. Equipped with a Bruker-X Flash-4010 EDX detector with a resolution of 133 eV (at the MnKα line), and a detector with sample holder to work in transmission mode (STEM-in- SEM).
  • Additional equipment in the “electron microscopy samples preparation laboratory” 

Contact
asuncion@icmse.csic.es
954 48 95 00 ext. 909211



Transmission Electron Microscopy




Scientific Responsibles
Dra. Asunción Fernández Camacho

Technical Assistant
Lda. Olga Montes Amorín, Dª. Inmaculada Rosa Cejudo


The transmission electron microscopy is a widely used technique for the microstructural and chemical characterization at micro and nanoscales, providing two-dimensional images of the sample texture and shape as well as grain and/or particle size, degree of homogeneity at the microscopic scale, degree of crystallinity of the sample, identification of crystalline phases, and high resolution images to identify the crystalline domains. The microscope is equipped with an EDX analyzer for compositional analysis. It can be applied to all type of materials and research topics in materials science and technology working with electron-transparent samples prepared ad-hoc for this end. The service performs transmission electron microscopy: Imaging in bright and dark field, selected area electron diffraction and high resolution electron microscopy, as well as elemental analysis of selected areas. It does not provide STEM mode. 

Available Equipment

  • JEOL 2100Plus microscope (200kV) with LaB6 filament. Structural resolution of 0.14 nm between lines and 0.23 nm between points. Sample holders with one and two angles. An X-ray Energy Dispersive Analyzer (EDX X-Max 80T, Oxford Instruments) and a CCD camera (Gatan) for image registration are attached to the equipment.
  • Additional equipment in the “electron microscopy samples preparation laboratory” 

Contact
asuncion@icmse.csic.es
954 48 95 00 exts. 909215 - 909216



Electron Microscopy Samples Preparation Laboratory




Scientific Responsibles
Dra. Asunciòn Fernández Camacho

Technical Assistant
Dª María Inmaculada Roja Cejudo, Dª Olga Montes Amorín (CicCartuja) , Dra. M. Carmen Jiménez de Haro


The laboratory for TEM and SEM samples preparation has a gold coater, a carbon evaporator, a metallization system for Cr and carbon, a diamond wheel cutter, a grinder with disc-grinder device, an ultrasonic cutter, a concave polishing (dimple) and ion thinning (Fischione 1010).


Contact
asuncion@icmse.csic.es
954 48 95 00 ext. 909216



Servicio de Difracción de Rayos X

X-Difracción Laboratory Service




Scientific Responsibles
Dr. Concepción Real Pérez

Technical Assistant
Ldo. José María Martínez Blanes


X-ray diffraction allows the qualitative and quantitative identification of crystalline substances and their microstructural and textural characterization.
At present, four independent diffractometers are available in this service, specifically config-ured to analyze the composition, chemical stability, crystallinity and many other properties in polycrystalline samples of a varied nature. Besides ordinary analyses (Θ-2Θ), part of the equipment can perform some advanced studies as:

  • Direct monitoring of transformations undergone in materials under heating, such as phase changes, under inert o reactive atmosphere.
  • To characterize materials at the nanoscale (1-100 nm) through X-ray scattering at low angles, using the SAXS technique.
  • To measure some physical parameters of layers such as density, thickness and surface rough-ness with the reflectometry setup.
  • To obtain the diffraction patterns of samples either sensitive to the atmosphere or highly transparent to X-rays (organic compounds) employing the capillary configuration.

Available Equipment

  • Diffractometer PANALYTICAL X’PERT PRO with automatic sample charger
  • Diffractometer PHILIPS X'PERT PRO with high temperature chamber (1200ºC) ANTON PAAR HTK 1200
  • Diffractometer PANALYTICAL X’PERT PRO (reflectometry, SAXS, low angle scattering and capillary)
  • Diffractometer SIEMENS D5000 DUAL (reflection and transmission)

Contact
creal@icmse.csic.es
954 48 95 49



Servicio de Análisis de Superficie

X-Ray Photoelectron Spectroscopy (XPS/ESCA)




Scientific Responsibles
Dr. Juan Pedro Espinós Manzorro, Dr. Juan Pedro Holgado Vázquez

Technical Assistant



Typically, “photoelectron spectroscopies” are a powerful set of non-destructive analysis techniques, exclusively sensitive to the more superficial few atomic layers (20-30 Å), allowing to obtain valuable information about their chemical, physical and electronic properties.

The technical interest of the resulting information is huge in fields such as catalysis, corrosion, surface treatments,, floating and adhesion phenomena, or segregation processes, among others. The most remarkable characteristic of X-Ray Photoelectron Spectroscopy (XPS/ESCA) is that it allows to discriminate, for a given element, between different oxidation states or chemical surroundings (coordination).
 

Available Equipment
Photoelectron Spectrometer VG ESCALAB 210, consisting on:

  • Analysis Chamber, equipped with a hemispheric multichannel analyser VG ESCALAB 210, a four axis manipulator, a dual X-ray source (achromatic Al Kα, Mg Kα), a UV lamp, and a electron gun, allowing to perform surface analysis by XPS, UPS and REELS, including angular resolved studies.
  • Two prechambers for different treatments, with ultimate vacuum levels of 10-8 and 10-9 mbar respectively, where samples can be subjected to diverse treatments and transferred to the analysis chamber without exposure to the atmosphere. The possible treatments include heating at high temperature (< 800C) under controlled atmosphere, ion sputtering with inert or reactive gases, exposure to plasma, laser treatments, deposition of metals, oxides or simple compounds, exfoliation, etc.

Photoelectron Spectrometer SPECS, consisting on:

  • Analysis Chamber, equipped with a hemispheric multichannel analyser PHOIBOS 100, three axis manipulator and dual X-ray source (achromatic Al Kα, Mg Kα).
  • Pre-chamber for High Pressure/High Temperature treatments (HPHT Cell).Samples can be subjected to treatments in the presence of gases up to 20 bar and 800ºC (simultaneously). These treatments can be performed either under static or flowing gas conditions. After treatments, samples can be transferred to the analysis chamber without exposure to the atmosphere.
  • A Fast entry chamber, equipped with a parking and degassing system, allowing the samples to be evacuated at moderate temperature (T < 150ºC). It is also possible to sputter the samples under an accelerated ion beam (0.5- 5.0 kV) using inert or reactive gases. Incorporation of some other equipment (Visible light illumination, metal evaporators) is also contemplated.

Contact
jpespinos@icmse.csic.es, holgado@icmse.csic.es
954 48 95 31 - 954 48 95 36



Servicio de Mecanizado

Mechanized Workshop




Scientific Responsibles
Dra. Ana Isabel Becerro Nieto

Technical Assistant
D. Juan Carlos Martín Sánchez, D. Manuel Perea Domínguez


The Machining workshop is a basic and essential service that provides technical support to the maintenance, change, fitting and development of simple scientific equipments, according with the current requirements of the experiments and projects carried out by the researchers at the ICMS.

Available Equipment
Besides other minor tolos for cutting, soldering, folding, drilling, etc, this workshop is equipped with:

  • CNC toolrom mill, HAAS TM 1P
  • Vertial toolrom, ERLO TSAR32
  • Toolrom mill EMCO F1P
  • Electronic lathe PINACHO SC200
  • Electronic lathe PINACHO SMART TURN180

Contact
jcarlos.martin@csic.es
954 48 95 00 ext. 909617



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