Thiophene fluorination to enhance photovoltaic performance in low
band gap donor –acceptor polymers.
Zhuping Fei
‡a
, Munazza Shahid
‡a
, Nir Yaacobi-Gross
b
, Stephan Rossbauer
b
, Hongliang Zhong
a
,
Scott E. Watkins
c
, Thomas D. Anthopoulos
b
, Martin Heeney*
a
Experimental section:
General: Reagents and chemicals were purchased from Aldrich and Acros unless otherwise
noted. 9-(Bromomethyl)nonadecane (1)
1
, 3,3’-Dibromo-5,5’-bis(trimethylsilyl)-2,2’-bithiophene
(4)
2
, (5-Bromo-3,4-difluoro-thiophen-2-yl)-trimethyl-silane (7)
3
and 4,7-Bis(5-bromo-2-thienyl)-
2,1,3-benzothiadiazole (11)
4
were synthesized by the reported method. Commercial 2,1,3-
benzothiadiazole-4,7-bis(boronic acid pinacol ester) (8) was purified by chromatography over
silica gel (eluent: 3% ethyl acetate in hexane), followed by recrystallisation from hexane before
use.
All reactions were carried out under Ar using solvents and reagents as commercially
supplied, unless otherwise stated.
1
H and
13
C NMR spectra were recorded on a Bruker AV-400
(400 MHz), using the residual solvent resonance of CDCl
3
or d-1,1,2,2-tetrachloroethane and
are given in ppm. Number-average (Mn) and Weight-average (Mw) were determined by Agilent
Technologies 1200 series GPC running in chlorobenzene at 80°C, using two PL mixed B
columns in series, and calibrated against narrow polydispersity polystyrene standards.
Preparative GPC utilised a Shimadzu recycling GPC system running in hexane at 40°C or
chlorobenzene at 80°C, using Agilent PLgel 10µm 50A or MIXED-D column, DGU-20A3
Degasser, LC-20A Pump, CTO-20A Column Oven andSPD-20A UV Detector. Electrospray
mass spectrometry was performed with a Thermo Electron Corporation DSQII mass
spectrometer. UV-vis spectra were recorded on a UV-1601 Shimadzu UV-vis spectrometer.
Flash chromatography (FC) was performed on silica gel (Merck Kieselgel 60 F254 230-400
mesh). Photo Electron Spectroscopy in Air (PESA) measurements were recorded with a Riken
Keiki AC-2 PESA spectrometer with a power setting of 5nW and a power number of 0.5.
Samples for PESA were prepared on glass substrates by spin-coating. Thermogravimetric
analysis (TGA) was carried out using a Perkin Elmer Pyris 1 TGA machine, with heating from
100 to 700°C, in dry air, at a heating rate of 10°C/min. Differential scanning calorimetry (DSC)
measurements: ~4 mg material was used for the DSC experiments, which was conducted under
nitrogen at scan rate of 20 ˚C min
-1
with a TA DSC-Q20 instrument.
OFET (organic field effect transistors) devices fabrication:
Bottom-gate, bottom-contact OFETs were fabricated on Si/SiO
2
substrates with
photolithographically patterned gold electrodes. The electrodes were again treated with the
pentafluorobenzene thiol SAM and the SiO
2
was treated with an octadecyltrichlorosilane (OTS)
SAM. The channel width and length of the transistors are 1.5 mm and 20 µm, respectively. The
polymer was dissolved in dichlorobenzene (5 mg/ml) at 100°C and spin cast to 100 °C
Electronic Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2012