solution of C
60
dissolved in benzene or toluene with
a concentration of 1 to 4 mmol /l. Then heating the
mixture under reflux under a nitrogen atmosphere
for 2 to 3 days. Then rinsing the samples obtained
with the pure solvent in order to remove the
physiosorbed C
60
molecules. The deposition of the
PCBM is carried out on the surface of a silica
substrate in order to measure the thickness by
ellipsometry, formed layers that can be calculated
from the following formula:
(6)
M: Number of oscillations.
: Wavelengths of the light passing
through the solution and the substrate.
and
indices of refractions of the
two mediums as a function of
.
The experimental measurement of the thickness
results in the value
. This shows that the
growth is carried out by 4 layers from bilayers.
Also the thickness can be measured by visible
UV absorption spectrophotometry by applying the
Beer-Lambert law:
(7)
Where A is the absorbance, α coefficient of
absorption of the layer vis-a-vis the radiation, ρ the
density of the layer, d the thickness of the studied
layer.
The covalent grafting between PCBM and C60
fullerene leads to changes in the absorption and
luminescence spectra of PCBMs that can be
characterized by Fourier Transform Infrared
Spectroscopy (FTIRS), so the evolution of the
substrate layer can be followed by surface-excited
Raman spectroscopy (SERS), this grafting is
manifested by the appearance of the characteristic
absorption bands in the infrared. For the visible UV
spectrum, we observe the appearance of a single
absorption band and this reveals a small amount of
C60 presented on the layers of PCBM. The quantity
of molecules on the surface remains constant as
shown by ESCA (electron spectroscopy for chemical
analysis) studies.
The stereochemistry of PCBMs is studied in 2D
((1H) and (13) C) NMR solutions in Deuterated
solvents (CDCl3, CD2Cl2) and the morphology of
the layer is characterized by Atomic Force
microscopy.
The mass percentages of C60 in the PCBM are
determined by thermogravimetric analysis from the
mass-temperature diagrams from which the different
degradation temperatures of the compound can be
derived. Concerning the P3HT crystallization
exotherms, the fusion endotherms are obtained by
the differential scanning calorimetry as well as the
melting and crystallization temperatures of the
P3HT:
and
The thermal effects of crystallization and
melting, the heating curves and those of the two
materials were studied by microcalorimetry(
and
) and the
differential thermal analysis, as well as the
crystallinity index of P3HT expressed by:
(8)
Or
: The enthalpy of fusion.
The reference enthalpy.
3 CHARACTERIZATION AND
ORGANIZATION OF THE
ACTIVE LAYER P3HT-PCBM
3.1 Organization of Polymer Chains
P3HT
The solubilization of P3HT in chlorobenzene is
dependent on the purity of the polymer, its high
molecular weight which can reach 50000 g / mol,
the stoichiometry, the chemical coupling conditions
(catalyst type, quantity and concentration) the
reaction conditions (1). absence of oxygen, good
magnetic or mechanical stirring) and finally the
solubility of the monomer and the polymers in the
reaction solvent. And in order to lead to a strong
fibrillar organization of the P3HT chains in the form
of a network leading to a high value of current
density, it is necessary that the interaction between
the polymer chains is more intense than their
interaction with the solvent. This aggregation of
chains in fibrillar structure is governed by
(π_stacking) and conditioned by the structure and
the chemical nature of the polymer, the interchain
interactions (hydrogen bonds, π interactions, dipolar
interactions...), solute solvent interactions and finally
the interactions of the substrate surface with the
polymer chains. The solvent of choice used for
structuring chains on fibrils is p-xylene.
(
)
which completely dissolves P3HT. At a temperature
of 80°C. For a concentration ranging from 0.5% (wt)
to 3% (wt) for one hour, which leads to an
organization of the chains or fibrils under low
temperature
for 4 hours in the
dark, the detection of these fibrils is carried out by
Physico-chemical Characterization, Structuration and Morphology of Photo-active Heterojunction (P3ht-Pcbm) Used In Organic
Photovoltaic Cells
221