Milli-Q water (resistivity 18.2 MΩ cm at 25 °C) was used in all experiments. PTA (99.995%) and potassium permanganate (KMnO4, >99.0%), sodium citrate, sodium chloride, bis(p-sulfonatophenyl)-phenylphosphine (BSPP, 97%), agarose and tetrachloroauric(III) acid (99%) were purchases from Sigma-Aldrich and used without any further purification. Gasket and O-rings for sealing of the liquid cell, PTFE tubings as well as small and large Poseidon E-chips were obtained directly from Protochips Inc21 . All used small E-chips had e-beam-transparent SiN membranes of nominal 550 μm × 20 μm expansion and flow spacers with 150 nm thickness (serial number: EPB-52DNF). As large E-chips, standard EPT-55W were used. RIE etched chips were obtained from Protochips company in the frame of a collaborative project. These modified chips are not catalog products but can be commercially requested from the company as of now. A possible fabrication routine is described in the physical prototyping of diffusion cells section. Two different LP-TEM sample holder setups, Poseidon Select™ and Poseidon 200™ (both Protochips Inc21 ), were used for experiments. All glassware was cleaned with aqua regia and rinsed thoroughly with Milli-Q water.
Poseidon select
Manufactured by Protochips
Sourced in United States
The Poseidon Select™ is a specialized piece of lab equipment designed for in-situ liquid-phase transmission electron microscopy (TEM) studies. It provides a controlled environment for observing dynamic processes at the nanoscale, enabling real-time visualization of liquid-based samples.
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2 protocols using poseidon select
1
In Situ Liquid Cell TEM Protocol
2
In-situ Liquid Cell TEM Observation
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The experiment was carried in a commercially available silicon nitride liquid cell electron microscope system (Poseidon Select, Protochips Inc., U.S.A.), as shown in Figure 1(i). It is an insitu electron microscopy platform which allows direct observation of liquids in TEM. In our study, 150 nm thick water film was sandwiched between two silicon based environmental chips (e-chips used: large e-chip (EHT-45ZZ, Protochips Inc., U.S.A.); small e-chip (EPB-55DS, Protochips Inc., U.S.A.)). These e-chips have a 50 nm thick silicon nitride (SiNx) windows suspended through a trapezoidal prism cavity of base dimensions 550 µm 50 µm for the in-situ observation. The echips were hydrophilized using a glow discharge plasma reactor (PIB-10, Vacuum Devices, Japan) before their assembly in the liquid cell holder. Moreover, the e-chips were assembled in crossaligned configuration so that their windows were perpendicular to each other and the available observation area was 50 µm 50 µm. This was done to minimize the window bowing during the TEM observation. After assembling the liquid cell, it was kept in a vacuum pumping station (10 -
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