Characterization of Graphene

1. Raman spectroscopy

Graphene platelets structure and coatings characterization

The obtained graphene nanoplatelets samples were characterized by an FE-SEM Supra 35 VP

scanning electron microscope coupled with an Oxford EDS system.

Raman spectra of the synthesized graphene nanoplatelets were obtained by a WITec Alpha 300
RAS Raman spectrometer.

Transmission and scanning transmission electron microscopy (TEM, STEM) micrographs were
obtained with a probe Cs – corrected JEOL JEM ARM – 200 CF microscope operating at
80 keV. Electron energy loss spectroscopy (EELS) was used for chemical analysis and thickness
determination. A Dual-EELS Quantum ER from Gatan was used to collect EELS spectra.

Atomic force microscopy (AFM) was carried out with graphene deposited on a Si wafer. The
AFM's AC mode was used to acquire images over the range 5 × 5 µm2 with the WITec Alpha
300 RAS.

Thermogravimetric analysis (TGA) was coupled with mass spectrometry with a Netzsch STA
449 F3 Jupiter instrument and a Netzsch QMS 403 C Aëolos spectrometer using the evolved gas
analysis method (EGA). The Experiment used a temperature scanning rate of 2 °C/min, a
temperature range of 20–850 °C, and N2 as an inert purging gas.

The coating thickness and the distribution of the pigment particles and graphene nanoplatelets
were determined by Focused Ion Beam Microscopy (FIB), using a FEI Helios Nanolab650
microscope coupled with an Oxford EDXS system and an X-max SDD detector.

IR spectra were collected using Fourier Transform infrared spectroscopy (FT-IR) with a Bruker
IFS 66/S spectrophotometer with a resolution of 4 cm−1, equipped with an integrating sphere
(OPTOSOL) and using a gold plate as a standard for diffuse reflectance.

UV–Vis spectra of the sol-gel spectrally selective coatings were obtained by a PerkinElmer
Lambda 950 UV–Vis spectrometer equipped with an integrating sphere.

The corrosion inhibition effect of graphene was measured with a Autolab PGSTAT30
potentiostat-galvanostat. Potentiodynamic (PD) polarization measurements were made in a
K0235 flat cell (Princeton Applied Research) filled with 0.5 M NaCl electrolyte. The coating on
an Al substrate was mounted as the working electrode. The reference electrode was Ag/AgCl
with saturated KCl and the counter electrode was a Pt grid. Before the linear sweep voltammetry,
the coatings were held at the open circuit potential for 30 min. For the potential sweep from − 1.0
to 0.0 V/Ag/AgCl/KCl, a scan rate of 0.5 mV/s was applied. The corrosion current density
(Jcorr) was extrapolated using the Tafel slopes from the potentiodynamic polarization curves.
However, this extrapolation has been shown to be an unideal method for evaluating the
effectiveness of corrosion inhibition [59], [60], [61].

Furthermore, the corrosion inhibition behaviour was tested using a salt chamber test by the
ASTM B117 standard. Samples were measured after 24 h of exposure, 72 h, 144 h and 211 h
(1 day, 3 days, 6 days and almost 9 days).

2.6. Determination of spectral selectivity

The coatings were analyzed for their spectral selectivity properties. This was determined from
the spectroscopic measurements. Solar absorptivity (aS) and thermal emissivity (eT) values were
determined from the reflectance spectra with the use of the procedure described in literature [62].
The aS is theoretically defined as a weighted fraction between absorbed radiation and incoming
solar radiation. This was calculated according to [62]:

(1)
where λ is wavelength, R(λ) reflectance in solar spectral region and S(λ) is solar spectrum with
air mass 1.5 (ISO standard 9845-1(1992)). Thermal emissivity eT is a weighted fraction between
emitted radiation and the Planck black body radiation r(λ,T) at absolute temperature T [62]:
(2)

The eT values were determined at the 350 K, with the aim to obtain values near the operating
temperature of the solar collectors.
From Soldano:

1. Atomic force microscopy (AFM)

2. Angle-resolved photoemission spectroscopy (ARPES)

3. Raman scattering

4. Rayleigh scattering