Laser Induced Breakdown Spectroscopy (LIBS)

Laser Induced Breakdown Spectroscopy (LIBS) is a material analysis technique exploiting the composition determination of the plasma induced during the laser ablation process. Due to the versatility of the ablation process, which allows the “vaporization” in the form of plasma (plasma plume) of any solid material, no preparation of the sample under analysis is required. Thanks to the size of the spot of the incident laser (10s-100s m) it is possible to perform compositional analyses having good spatial resolution both lateral (x, y) and vertical (z: stratigraphic analysis).

LIBS@ns LIBS@fs
   

 

Gas chromatography (GC)

Gas-Chromatography is an analytical technique which allows to separate and to quantify the components of an organic products mixture. The identification of such components can be obtained by comparison with authentic samples.
This technique is usually applied to show the results of a reaction under investigation by separating and quantifying reactants from products, in order to evaluate the effects of the experimental conditions on activity and selectivity. The mixture has to be solved in a solvent and injected in the gas-chromatograph. All the components are eluted through the capillary column with different velocity and the they pass through the detector giving as final result a graph reporting Intensity Vs. time. The choice of the column and of all the analysis parameters (i.e.: programmed Temperature Vs. time) allows the separation and quantification of compounds with very similar chemical characteristics.

GC Agilent 6850

Electrospray ionisation (ESI)

The Electrospray Ionization (ESI) technique allows to bring molecules and compounds like biomolecules, nanoparticles and complexes as intact and isolated charged units in the gas phase.
Mass spectrometry, is a powerful tool for a variety of analytical applications and is ideally suited for the preparation of charged molecules with well-defined compositions and charge state. The combination of an ESI-source and a set-up for mass spectrometry in the custom-made instrument under construction at ISM will allow to select and deposit mass- and charge-selected ions of several different materials on surfaces.
The ESI source operates at ambient pressure and the produced molecular ions are transported in vacuum via a differential pumping section. A system of electrostatic lenses and an octupole remove most of the contaminations from neutral species and solvent molecules, transporting the ion beam into a quadrupole mass filter (QMS), operated in high vacuum, which performs the mass/charge selection. An electrostatic deflector then directs the beam either to a characterization section or to a “soft-landing” deposition chamber. A third line for gas phase spectroscopy will be implemented in the near future. 

ESI

Electrochemical analysis

Electrochemical analysis uses electrically conductive probes or electrodes which are usually linked to electronic devices that measure the electrical parameters generated by the redox reaction of the species in solution. The electroanalytical techniques usually use three electrodes, known as the working electrode, the reference electrode and the counter (auxiliary) electrode. These electrodes are connected to a potentiostat that controls the working electrode potential and determines the resulting current providing information about the electrical parameters of the reactants in solution.
Cyclovoltammetry
The Cyclovoltammetry (CV) is an electrochemical technique based on the application of a potential to a stationary electrode immersed in an unstirred solution. In a common experiment, a variation of potential is imposed on a working electrode and the contextual variation of current is recorded. The potential varies linearly with a speed called" scan speed", generally measured in volts per second (V / s). The measuring cell typically has 3 electrodes immersed in the solution of the electroactive compound and a supporting electrolyte. The potential is measured between the reference electrode, with constant potential, and the working electrode, while the current is measured between the working electrode and the counter electrode; the current (i) is reported against the applied potential (E) to give the so-called cyclevoltammogram. As the potential changes for each compound that can be reduced (or oxidized) there will be an exchange of electrons with the working electrode, so as to give a variation of the measured current which produces a peak in the voltammogram. If the process is reversible, by inversion of the applied potential, the product formed in the first part of the scan will be re-oxidized (or reduced) producing a current of opposite polarity. The new peak of the voltammogram will have a shape similar to the previous one but with reverse polarity. From this it is possible to derive the redox potential and the speed of the electrochemical reaction that took place. 
PalmSens4 Autolab PGStat 204

Chemical synthesis-characterization

Laboratory chemical synthesis-characterization

Anna Maria Paoletti  - annamaria.paoletti@ism.cnr.it

BC11@Mlib

 
  • electrochemical characterization techniques
  • voltammetric techniques
  • electrochemical impedance spectroscopy techniques EIS
  • resistivity measurements with pneumatic four points probe, interfaced with Keithley 236 source measure unit
 

TECHNICAL SPECIFICATIONS

Potenziostato-galvanostato

  • Autolab PGStat 204 con modulo FRA 32M per EIS Metrohm (2014)
    • Potential range    +/- 10 V
    • Compliance voltage    +/- 20 V
    • Maximum current    +/- 400 mA
    • Current ranges    100 mA to 10 nA
    • Potential accuracy    +/- 0.2 %
    • Potential resolution    3 µV
    • Current accuracy    +/- 0.2 %
    • Current resolution    0.0003 % (of current range)
    • Input impedance    > 100 GOhm
    • Potentiostat bandwidth    1 MHz
    • Computer interface    USB
    • Control software    NOVA

Four-point measures

  • Alessi 645 Four Point Wafer base Probe, interfaccia con Keithley 236 source measure unit

AVAILABLE TECHNIQUES

  • Ciclovoltammetria (CV)
  • Electrochemical impedance spectroscopy techniques (EIS)
  • Resistivity measurements with pneumatic four points probe, interfaced with Keithley 236 source measure unit
 

SAMPLE

  • Solutions (min concentration 10-4M, min volume 5-10 ml) or films on conductive substrates

USE FOR

  • Characterization of electroactive materials