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The present invention relates to a liquid phase transmission electron microscopy (LP-TEM) holder with integrated temperature regulation for operating with an associated transmission electron microscopy instrument providing an electron beam for imaging, the LP-TEM holder comprising a liquid phase sample receptacle (LPSR, 5) which may be made from two or more layers of materials, e.g. microchips, the LPSR providing a liquid compartment. The LP-TEM holder furthermore comprises an integrated temperature regulating unit (15), capable of regulating the temperature of the LPSR and liquid in the liquid compartment by means of a temperature measuring unit (16) capable of measuring a temperature in the liquid compartment. The LPSR is thermally isolated with a thermal isolating portion (30), with respect to an external environment and associated devices. The invention is particularly advantageous for providing fast temperature regulation and accurate steady state temperatures of one or more fluids to be imaged.

Liquid phase transmission electron microscopy (LPTEM) is rapidly developing as a powerful tool for probing processes in liquid environments with close to atomic resolution. Knowledge of the water thickness is needed for reliable interpretation and modelling of analytical studies in LPTEM, and is particularly essential when using thin liquid layers, required for achieving the highest spatial resolutions. The log-ratio method in electron energy-loss spectroscopy (EELS) is often applied in TEM to quantify the sample thickness, which is measured relative to the inelastic mean free path (λIMFP). However, λIMFP itself is dependent on sample material, the electron energy, and the convergence and divergence angles of the microscope electronoptics. Here, we present a detailed quantitative analysis of the λIMFP of water as functions of the EELS collection angle (β) at 120 keV and 300 keV in a novel nanochannel liquid cell. We observe good agreement with earlier studies conducted on ice, but find that the most widely used theoretical models significantly underestimate λIMFP of water. We determine an adjusted average energy-loss term Em, water, and characteristic scattering angle θE, water that improve the accuracy. The results provide a comprehensive knowledge of the λIMFP of water (or ice) for reliable interpretation and quantification of observations in LPTEM and cryo-TEM studies.

Liquid-phase transmission electron microscopy (LPTEM) offers label-free imaging of nanoparticle (NP) processes in liquid with sub-nanometer spatial and millisecond temporal resolution. However, LPTEM studies have reported only on NPs moving orders of magnitude slower than expected from bulk aqueous liquid conditions, likely due to strong interactions with the LPTEM liquid-enclosing membranes. We demonstrate how scanning transmission electron microscope (STEM) imaging can be used to measure the motion of individual NPs and agglomerates, which are not hindered by such interactions. Only at low electron flux do we find that individual NPs exhibit Brownian motion consistent with optical control experiments and theoretical predictions for unhindered passive diffusive motion in bulk liquids. For increasing electron flux, we find increasingly faster than passive motion that still appears effectively Brownian. We discuss the possible origins of this beam-sample interaction. This establishes conditions for the use of STEM as a reliable tool for imaging nanoscale hydrodynamics in situ TEM.

Improving our experimental and theoretical knowledge of electric potentials at liquid-solid boundaries is essential to achieve a deeper understanding of the driving forces behind interfacial processes. Electron holography has proved successful in probing solid-solid interfaces but requires knowledge of the materials’ mean inner potential (MIP, V0), which is a fundamental bulk material property. Combining off-axis electron holography with liquid phase transmission electron microscopy (LPTEM), we provide the first quantitative MIP determination of liquid water V0 ¼ þ4.48 0.19 V. This value is larger than most theoretical predictions, and to explain the disagreement we assess the dominant factors needed in quantum simulations of liquid water. A precise MIP lays the foundations for nanoscale holographic potential measurements in liquids, and provides a benchmark to improve quantum mechanical descriptions of aqueous systems and their interfaces in, e.g., electrochemistry, solvation processes, and spectroscopy.