Harris et al. ESI: Ultra-smooth mineral films 1/6
Electronic Supplementary Information
Ultra-smooth and space-filling mineral films generated via
particle accretion processes
Joe Harris, Ingo P. Mey, Corinna F. Böhm, Thi Thanh Huyen Trinh, Simon Leupold, Carsten Prinz,
Philip Trippal, Ralf Palmisano and Stephan E. Wolf*
* To whom correspondence should be addressed: stephan.e.wolf@fau.de
Experimental Details
Materials
Sodium poly(acrylate) Mw 5100 (Fluka),
calcium chloride 1.0 M solution (Carl Roth),
magnesium chloride hexa-hydrate (Sigma
Aldrich), 2-(N-morpholino) ethanesulfonic acid
and fluorescein glycine amide (Thermofisher
Scientific), 1-ethyl-3-(3-dimethylaminopropyl)
carbodiimide (Sigma Aldrich), hydrochloric
acid (Carl Roth) and ammonium carbonate
(Carl Roth) were used as received without
further purification. Glassware was cleaned
with deionised water, immersed in 1 M HCl for
5 minutes and subsequently rinsed with
deionised water before air drying.
Film preparation by
slow-diffusion mineralization
In a typical experiment, film precipitation was
performed in a closed 21 litre volume desiccator
at 25 °C for 42 hours.[1] A 9 cm diameter petri
dish was used as a crystallisation vessel. This
contained 25 ml of a 10 mM CaCl2, 0 to 15
mM MgCl2·6H2O, 200 μg ml-1 PAA solution.
The petri dish was covered with clingfilm
which was punctured with one 1 mm diameter
needle hole, this was sealed in a desiccator with
two glass vials (10 ml) each containing 3g of
freshly crushed ammonium carbonate powder.
Each vial was covered with parafilm punctured
with a single 1 mm diameter needle hole placed
at the bottom of the desiccator. The number of
glass vials bearing ammonium carbonate or,
alternatively, the number of needle holes in the
vial(s) affect the escape rate of carbon dioxide
and ammonia released from the decomposing
ammonium carbonate powder to the
desiccator’s gas phase This provides a very
simple but efficient control over the rate by
which the composition of the gas phase is
saturated with respect to carbon dioxide and
ammonia. This, in turn, affects the rate of
ammonium carbonate uptake in the reaction
solution, eventually controlling the pH and
supersaturation profile of the reaction.
Alternatively, the desiccator size can be altered;
see Harris et al. (2017) for more details [1].
The films were recovered from solution,
rinsed with ethanol, and air dried. The defect-
free films could be easily extracted from the
interface using a microscope coverslip; optical
microscopy under cross-polarization, FT-IR,
and XRD analyses indicated absence of
crystalline polymorphs in case of Mg-doped
films.
Preparation of fluorescein glycine
amide-tagged PAA
A 2.5 mg ml
-1
sodium poly(acrylate) was prepared
in a 100 mM MES buffer at pH 4.9. A 4 ml volume
of this solution was used to dissolve 1 mg
fluorescein glycine amide. A volume of 0.1 ml of
EDC solution (0.19 M) in MES buffer at pH 4.9
was added to the sodium poly(acrylate)/fluorescein
glycine amide solution. The reaction was stirred for
4 hours in the dark to yield fluorescein-labelled
poly(acrylate). Unreacted EDC and fluorescein
glycine amide, and buffer molecules were removed
by dialysis (Mw cut off 3500 Da) against deionized
water for 48 hours in the dark with regular changes
Electronic Supplementary Material (ESI) for Nanoscale Horizons.
This journal is © The Royal Society of Chemistry 2019