Title: Wafer-scale fabrication of mesoporous silicon functionalized with electrically conductive polymers, XRD and electrochemical datasets
DOI: https://doi.org/10.15480/882.9049
Author: May Manfred, manfred.may@tuhh.de, Technical University Hamburg, https://orcid.org/0000-0002-4015-232X
context: This datasets were generated during the synthesis and characterization of hybrid materials made out of a mesoporous silicon host and conductive polymers (PANI,PPy and PEDOT).
The envisioned application is that of an hybrid thermoelectric material following the electron-crystal-phonon-glass approach.
methods:
electrochemical synthesis:
All electrochemical polymerization experiments are conducted using a custom-built teflon-based polymerization cell. The cell consists of a platinum mesh counter electrode (CE), an
Ag/AgCl reference electrode (RE, Sensortechnik Meisenberg), and mesoporous silicon epilayers serve as the working electrodes (WE). All electrodes are connected to a potentiostat (Metrohm-Autolab
PGSTAT 30). The polymers PPy and PEDOT are synthesized out of a solution of 0.1 M monomer and 0.1 M LiClO4 in acetonitrile (ACN). For the galvanostatic production of the PEDOT/PPy/pSi
hybrids a current of 0.255 mAcm−2 is applied. The PANI polymer was synthesied according to the following composition: 0.25 M Aniline in 3 M EtOH (aq) and 1 M HCl. When applicable, data is normalized to the substrate area in con-
tact with the solution, without considering the increased surface area due to the porosification of the silicon = 7.86cm². This approach was chosen due to the unknown active surface area of the pSi and the
assumption that the pore ends are the preferred sites of polymerization initiation.
X-ray diffraction:
The powder diffraction (PXRD) samples (Fig.6a) are measured at a Bruker D8 Advancedevice with copper radiation of 0.154 nm wavelength in the Θ − Θ geometry.
The synchrotron-based scattering experiments conducted at the beamline P08 of PETRA III (DESY) on solid state polymerized (SSP) PEDOT/pSi hybrids. The incoming beam
(E = 25 keV) hits the sample and is scattered onto the 2D detector. To check whether preferred orientation of the organic species in the mesoporous pore space occurs the sample can
be rotated from ω = 0 − 90 ° (here 0°, 25°, 50° and 75°). At ω = 0 ° the pore axis are parallel to the incoming beam, at higher omega values increasingly perpendicular. 
For peak fitting (Fig. 6c. inset) the free software LIPRAS (North Carolina State University) is used. Typically a Pseudo-Voigt fit gives the best result. The samples
used for the in-situ measurements during SPP of DBEDOT to PEDOT in mesoporous silicon are freshly prepared onsite in order to inhibit polymerization at room temperature. The experiments
are conducted in a homemade sample cell under nitrogen atmosphere at 60 °C.
Data structure:
Fig.1 to Fig.4 contains the electrochemical datasets of the synthesis of different conductive polymers on a silicon substrate in the .txt format. CV measurements --> plot current against voltage, galvanostatic --> plot voltage against time,
potentiostatic --> plot current against time
Fig.6a are .txt files of the PXRD measurements of DBEDOT, PEDOT and PEDOT EtOH rinsed. --> plot counts against the 2-theta value for a regular diffractogram.
Fig.6c and Fig.6d contains 2D detector images recorded at the P08 Beamline/DESY. One dataset consits of a dataset recorded during SSP (Fig.6c, T=60°C, t=0-6hours), the second dataset the impact of rotation angle omega. 
Additionally a .png file of the detector parameters is given and a calibration file of LaB6 measurement. Use appropriate software in order to view the datasets (Fit2D etc.).
Terms of Use:
All data is free to use.