University of the Basque Country University of the Basque Country

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COUPLED MULTISPECTROSCOPY SINGULAR LABORATORY (Raman-LASPEA)

Equipment

The Singular Coupled Multispectroscopy Laboratory (Raman-LASPEA) has the following equipment:

  1. Confocal Raman Microscope
    • Three excitation lasers: 325, 514 and 785 nm
    • Ability to perform both puntual measurements as surface analysis by Raman image
    • Two external optical fiber probes allow analysis of macrosamples and a Linkam TS1500 temperature platform, obtain spectra of compounds at high temperatures
  2. FTIR Spectrometer and microscope
    Analysis in transmission mode, diffuse reflectance (DRIFT) and attenuated total reflectance (ATR) either occasionally as by imaging.
  3. SEM Electron Microscope
  4. Microanalysis equipment thru dispersion of energies EDS
  5. Structural Chemistry Analyzer (SCA)
    We can get from a sample the following information:
    • Morphology (secondary electrons image)
    • Information on the composition (average atomic number in the backscattered electron image)
    • Elemental composition (EDS spectrum)
    • Chemical composition and identification (Raman)
    • Electronic structure (PL)
    • Physical structure and properties (mechanical and crystallographic data)
  6. Atomic Force Microscope (AFM-Raman and TERS)
    Analysis at nanoscale and Raman amplification of the signal in a very targeted area of the sample.

Raman confocal microscope

This is an InVia Raman confocal microscope made by Renishaw, comprising a spectrometer and two lasers coupled to a Leica optical microscope. The excitation wavelengths of the lasers are 514 nm (green) and 785 nm (NIR), which enables analyses to be carried out using two different sources of energy, thus increasing the options for successful analysis and enabling possible fluorescence-based phenomena to be avoided. The spectrometer is equipped with two different modular optics depending on the laser being used. In all cases, a spectral resolution of 1 cm -1is obtained with a good signal-noise ratio.

For its part, the Leica microscope incorporates 5x, 20x and 50x lenses, enabling maximum performance to be obtained from the laser photons in order to increase the sensitivity of the equipment by increasing the Raman effect. The confocality also enables maximum lateral resolution of the microscope to be obtained. The microscope incorporates a motorized XY slide for greater comfort and so as to be able to carry out  Imagen Raman analyses.

The Leica microscope may also be used as an optical micrscope, with reflected light and transmitted, etc., thus enabling any observations to be saved in digital format thanks to the video camera incorporated. The whole unit is placed on an optical desk to prevent any possible vibrations.

FTIR spectrometer

The laboratory is equipped with an FTIR spectrometer made by Jasco (4200 model) for determining FTIR spectres in medium infrared (400-4000 cm-1 ) using the potassium bromide pellet technique. The spectral resolution attained by the equipment is 0.5 cm-1.

FTIR image microscope

The  FTIR spectrometer is coupled to an FTIR scanning microscope made by Jasco (IMV 4000 model) and with motorized slide for carrying out FTIR Image analysis. The spectroscopic range scanned is from 4000 tp 750 cm-1 (limit determined by ZnSe optics). Its 16-detector online matrix enables analyses to be carried out in very short periods of time. Analyses may be carried out both in reflectance mode (16x y 32x), and transmittance mode (16x y 32x), as well as in ATR (16x).

SEM microscope

The laboratory has Carl-Zeiss EVO-40 Electronic Scanning Microscopy equipment at its disposal, whereby both photography in high vacuum mode (with metallization of the samples) and in extended pressure or low vacuum and wet sample mode (without the need to metallize the samples) can be used.

The ewuipment features a secondary electron detector (SIM) and a retroscattered electron detector, together with an EDS elementary analyzer.

EDS microanalysis equipment

The labatory has EDS microanalysis equipment made by Oxford Instruments at its disposal, coupled to the camera of the SEM microscope, thus enabling elementary analyses of the samples observed in the microscope to be carried out.

The EDS equipment enables both specific analyses such as scanning and mapping to be carried out, thus also permitting the analysis of EDS image from both a qualitative and quantitative standpoint.

Auxiliary Equipment

In addition to the measurement equipment, the Service also has other auxiliary equipment for sample preparation or maintenance of certain conditions (environmental and electrical).

The first group includes a hydraulic press for the preparation of KBr tablets for the FTIR spectrometer, a stove or an Emitech K500x metallizer that allows the deposition of a thin layer of carbon or gold to render the surfaces of the samples they will observe / analyze using SEM-EDX  conductive.