Authors: E. Maaskant, K. Tempelman and N.E. Benes
Films in Fluids, Department Science and Technology, University of Twente

Corresponding author: N.E. Benes

Contact information:

n.e.benes@utwente.nl
University of Twente - Films in Fluids
P.O. Box 217
7500 AE Enschede
The Netherlands

***Figure 1:TGA***

*** General Introduction ***
This dataset includes the thermal gravimetric analysis (TGA) data in combination with mass spectroscopy data of Poly(PDMS-POSSamic acid) powders before and
after imidization. 
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
Combined thermogravimetric analysis (TGA) and mass spectroscopy (MS) measurements were performed on
poly(PDMS-POSSamic acid) powders using an STA 449 F3 Jupiter TGA with an aluminum sample cup (Netzsch,
Germany) and QMS 403 D Aeolos MS (Netzsch, Germany). Mass loss measurements were performed from 50
to 1000 C with a heating rate of 20 C min-1 under both air and nitrogen atmospheres. Isothermal analysis was
performed at 250 C with a heating rate of 10 C min-1 under nitrogen atmosphere.

*** Data specification ***
The excel files includes data on the mass loss (%) and on the Ion current strength for each component 
18.09 = H2O
16.09 = CH4
30.05 = NO
43.97 = CO2
42.97 = CH3CH2CH2


***Figure 2:Heat stage***
*** General Introduction ***
This dataset includes the raw measurement data and the modelled data of thin PDMS-POSS films on top of a Si wafer as function of a temperature profile. This
data shows the structural changes upon imidization of the PDMS-POSS amic acid film. 
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
M2000X spectroscopic ellipsometer (J.A. Woollam Co.) with focussing probes. 
The ellipsometry data for imidization was collected with a Linkam heating stage with quartz windows with an
incident angle of 70. The non-imidized films, used for imidization measurements with ellipsometry, were stripped of
residual solvents in a furnace at 110 C for 20 minutes. The temperature measurements were performed under ultra
pure N2 at a flow rate of 100 mL min-1. A temperature correction was performed according to the procedure described
by Kappert et al.(the difference between set point and actual temperature was less than 1 C). Prior to heating, the
samples were flushed at 25 C under N2 flow for 30 minutes. Then, the samples were heated to 250 C at 5 C min-1
and remained at 250 C for 20 minutes. The samples were cooled down with a cooling rate of 20  C min-1.

The completeEase software from J.A. Woollam Co. was used to analyse the data.

*** Data specification ***
The files with a file extension .SE are the dry measurement inside the heatcell at 25degC.
The .iSE extention files include the temperature dependent measurements as function of time. 
The heat profile used is provided by the .tp file.


The excel sheet includes the modelled data and the calculated relative thickness and refractive index.

d_relative=d_t/d_0


***Figure 3:Swelling PDMS*** & ***Figure S4_refractive index_PDMS***
*** General Introduction ***
This dataset includes the raw measurement data and the modelled data of thin PDMS films (1:10 crosslinked, Permacol RTV 615 A/B) on top of a Si wafer in
hexane, ethyl acetate and ethanol. This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin highly cross-linked PDMS
films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
M2000X spectroscopic ellipsometer (J.A. Woollam Co.) with focussing probes. 
The ellipsometry swelling measurements were performed with a custom-built Teflon liquid flow cell with quartz windows with an incident angle of 70. 
The cell volume was 25.5 cm3. The cell temperature was controlled with an external water bath (LAUDA-Brinkmann, LP.), allowing water at 25 C to flow 
through the outer walls of the cell. The optical retardance of the windows of the measurement cell was corrected for using calibrated delta osets. The
solvent vapor flow was generated using two identical bubblers in series, both at 25 C. The carrier gas was a ultra pure N2 gas, with a gas flow of
100 mL min-1.

The completeEase software from J.A. Woollam Co. was used to analyse the data.

*** Data specification ***
The files with a file extension .SE are the dry measurements within the teflon cell. 
The .iSE extention files include the swelling measurements in the mentioned solvent vapour as function of time. 
The two calibration files include a measurement of a SiO2 25nm calibration wafer outside (ex-situ) and inside the teflon cell (in-situ). Using this data,
the window offset of the teflon cell could be determined. 

The excel sheet includes the modelled data (tabs including 'Full data' in tab name) and the calculated swelling degree and normalized refractive index data. 
The .mod extensions show the optical model used for the modelling. 

SD=(d_swollen/d_dry - 1)*100%

n_norm=(n_swollen-n_solvent)/(n_dry-n_solvent)



***Figure 4:Swelling PDMS-POSS*** & **Figure S5_Index_PDMS_POSS***
*** General Introduction ***
This dataset includes the raw measurement data and the modelled data of thin PDMS-POSS films on top of a Si wafer in hexane, ethyl acetate(EA) and ethanol.
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
M2000X spectroscopic ellipsometer (J.A. Woollam Co.) with focussing probes. 
The ellipsometry swelling measurements were performed with a custom-built Teflon liquid flow cell with quartz windows with an incident angle of 70. 
The cell volume was 25.5 cm3. The cell temperature was controlled with an external water bath (LAUDA-Brinkmann, LP.), allowing water at 25 C to flow 
through the outer walls of the cell. The optical retardance of the windows of the measurement cell was corrected for using calibrated delta osets. The
solvent vapor flow was generated using two identical bubblers in series, both at 25 C. The carrier gas was a ultra pure N2 gas, with a gas flow of
100 mL min-1.

The completeEase software from J.A. Woollam Co. was used to analyse the data.

*** Data specification ***
The files with a file extension .SE are the dry measurements within the teflon cell. 
The .iSE extention files include the swelling measurements in the mentioned solvent vapour as function of time. 
The calibration files include a measurement of a SiO2 25nm calibration wafer outside (ex-situ) and inside the teflon cell (in-situ). Using this data,
the window offset of the teflon cell could be determined. 

The excel sheets include the modelled data (tabs including 'Full data' in tab name) and the calculated swelling degree and normalized refractive index data. 

SD=(d_swollen/d_dry - 1)*100%

n_norm=(n_swollen-n_solvent)/(n_dry-n_solvent)



***Figure 5:Zetapotential***
*** General Introduction ***
This dataset includes the streaming current measurements of Poly(PDMS-POSSimide) films on top of a Si wafer. 
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
Streaming current measurements were performed on a SurPASS (Anton Paar, Austria) analyzer equipped with a
adjustable gap cell. Poly(PDMS-POSSimide) films were deposited on silicon wafers of 1  2 cm2. The wafers were
attached to the adjustable gap cell by double sided adhesive tape. The pH of the electrolyte solution (5 mM KCl)
was automatically adjusted using 0.1 M NaOH

*** Data specification ***
.txt file extensions include the data as obtained for two different samples.
.py provides the data compilation in Python.



***Figure 6:Permeation***
*** General Introduction ***
This dataset includes the ethanol permeation data at 20 bar of a Poly(PDMS-POSSimide) film on top of porous alpha-alumina disk coated with two layers of
gamma-alumina (pervatech, The Netherlands).
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
Ethanol permeation measurements were performed on a custom-built dead-end permeation setup. A feed vessel
was pressurized to 20 bar using ultra pure N2. Permeate streams were measured with a mass balance.

*** Data specification ***
The .lvm extension files include the permeation data at 20 bar for three different samples. These files can be opened in LabView.
The .py extention file is the file used to make the figure in Python. 



***Figure S1_FTIR_amic_acid***
*** General Introduction ***
This dataset contains the ATR-FTIR absorption data of a PDMS-POSS amic acid powder sample preapred at five different pH's (as can be found in the filename).
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of 
ultra-thin highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
ALPHA spectrometer (Bruker, Germany) in FTIR-ATR mode.



***Figure S2_FTIR_amic_acid_imide***
*** General Introduction ***
This dataset contains the ATR-FTIR absorption data of a PDMS-POSS amic acid powder sample before (PDMS_POSS_amic_acid_pH9_11.txt) and after 3 hours of imidization at 
230degC (PDMS_POSS_imid_230C_3h_pH9_11.txt). Python (FTIR_amicacid_to_imide.py) was used to make the final figure (PDMS_POSS_FTIR.pdf). This work is part of 
the publication 'Hyper-cross-linked thin polydimethylsiloxane films' (DOI:...) in which the preparation and performance of ultra-thin highly cross-linked PDMS
films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
ALPHA spectrometer (Bruker, Germany) in FTIR-ATR mode.



***Figure S3_TGA***
*** General Introduction ***
This dataset includes the thermal gravimetric analysis (TGA) data in combination with mass spectroscopy data of Poly(PDMS-POSSamic acid) powders in both air 
and nitrogen atmosphere.
This work is part of the publication 'Hyper-cross-linked thin polydimethylsiloxane films' in which the preparation and performance of ultra-thin 
highly cross-linked PDMS films by interfacial polymerization with polyhedral oligomeric silsesquioxane (POSS) is described. 

*** Test equipment ***
Combined thermogravimetric analysis (TGA) and mass spectroscopy (MS) measurements were performed on
poly(PDMS-POSSamic acid) powders using an STA 449 F3 Jupiter TGA with an aluminum sample cup (Netzsch,
Germany) and QMS 403 D Aeolos MS (Netzsch, Germany). Mass loss measurements were performed from 50
to 1000 C with a heating rate of 20 C min-1 under both air and nitrogen atmospheres. Isothermal analysis was
performed at 250 C with a heating rate of 10 C min-1 under nitrogen atmosphere.

*** Data specification ***
ExpDat_20150429_PDMSPOSS_pH911_20K_1000C_AIR_TG_TGAMSmerged.xls --> air atmosphere
ExpDat_20150506_PDMSPOSS_pH911_20K_1000C_N2_TG_TGAMSmerged.xls --> N2 atmosphere
ExpDat_20160728_PDMS_POSS_amicacid_isothermal_250C_TGAMSmerged.xls --> Isothermal at 250degC
The excel files includes data on the mass loss (%) and on the Ion current strength for each component 
18.09 = H2O
16.09 = CH4
30.05 = NO
43.97 = CO2
42.97 = CH3CH2CH2


