Spectroscopy Service

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

Reserva on-line

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

Atomic Emission Spectrometry (ICP-OES)

Scientific Responsibles
Dr. Francisco José Gotor Martínez

Technical Assistant
Lda. Belinda Sigüenza Carballo

Inductively coupled plasma atomic emission spectrometry (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
francisco.gotor@icmse.csic.es
954 48 95 40


Formulario ICP.docx

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

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 Rosa 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

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 PHOIBOS 100-DLD, consisting on:

• Analysis Chamber, equipped with a hemispheric multichannel analyser PHOIBOS 100-DLD, 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, ISS 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