Inhibition of vacuum sublimation artefacts for (Scanning) Transmission Electron Microscopy ((S)TEM) of sulphur samples via encapsulation

Lithium-sulfur battery is one of promising candidates for next-generation energy storage device due to the sulfur cathode material with low cost and nontoxicity, and super high theoretical energy density (nearly 2600Wh kg−1) and specific energy (2567Wh kg−1). Sulphur, however, poses a few interesting challenges before it can gain widespread utilisation. The biggest issue is known as the polysulphide shuttling effect which contributes to rapid capacity loss after cycling. Accurate characterisation of sulphur cathodic materials becomes critical to our understanding polysulphide shuttling effect in the quest of finding mitigating solutions. Electron microscopy is playing a crucial role in battery research in determining structure–property–function relations. However, sulphur undergoes sublimation at a point above the typical pressures found in the column of a transmission electron microscope (TEM) at room temperature. This makes the imaging and characterisation of any sort of nanostructured sulphur samples challenging, as the material will be modified or even disappear rapidly as soon as it is inserted into the TEM vacuum. As a result, materials characterised by such methods are prone to deviation from normal conditions to a great extent. To prevent this, a novel method of encapsulating sulphur particles between silicon nitride (SiNx) membranes is demonstrated in this work.

Ionic Liquid-Assisted Grinding: An Electrophilic Fluorination Benchmark

We demonstrated the influence of liquid additives on the rate and selectivity of mechanochemical fluorination of aromatic and 1,3-dicarbonyl compounds with F-TEDA-BF4. Substoichiometric catalytic quantities of ionic liquids speed up the reaction. We proposed an improved protocol for ionic liquids-assisted fluorination that allows easy and efficient isolation of fluorinated products by vacuum sublimation. A careful choice of additive results in high yields of fluorinated products and low E-factor for the overall process. Here, we report a benchmarking study of various ionic liquids in comparison with representative molecular solvents. A lower viscosity of ionic liquid additive is typically associated with higher yields and a higher degree of difluorination. Ionic liquids with fluorous anions (triflate and triflimide) are shown to be the most efficient catalysts for ionic liquid-assisted grinding.

Sublimation of organic-rich comet analog materials and their relevance in fracture formation

Aims. The morphology of cometary nuclei is the result of an ongoing evolution and can provide valuable information to constrain the composition of comets. In our laboratory experiments we investigated the morphological evolution of comet analog materials, which consist of volatile, dust, and organic components. The laboratory results are aimed to help understand the evolution of cometary surfaces. Methods. We used spherical particles of fly ash and mixtures of ice, glycine, and sodium acetate as analog materials in different mass ratios to reproduce observed cometary morphologies. The cohesive and gravitational properties in the laboratory are scaled to cometary conditions to draw meaningful conclusions from the experimental results. The samples were placed in a vacuum sublimation chamber, cooled down to below 150 K, and were insolated with an external light source. To analyze the morphology of the samples, a camera was used to monitor the alterations of the surface. Results. Organic components in volatile-rich samples can have a distinct adhesive effect after the volatiles sublimate. During the sublimation process the sample volume decreases and fractures form on the sample surface. Due to the stability of the remaining volatile-depleted material, significant cliff collapses or ejected particles were not observed in the laboratory.

Crystal structure of copper perchlorophthalocyanine analysed by 3D electron diffraction

Copper perchlorophthalocyanine (CuPcCl16, CuC32N8Cl16, Pigment Green 7) is one of the commercially most important green pigments. The compound is a nanocrystalline fully insoluble powder. Its crystal structure was first addressed by electron diffraction in 1972 [Uyeda et al. (1972). J. Appl. Phys. 43, 5181–5189]. Despite the commercial importance of the compound, the crystal structure remained undetermined until now. Using a special vacuum sublimation technique, micron-sized crystals could be obtained. Three-dimensional electron diffraction (3D ED) data were collected in two ways: (i) in static geometry using a combined stage-tilt/beam-tilt collection scheme and (ii) in continuous rotation mode. Both types of data allowed the crystal structure to be solved by direct methods. The structure was refined kinematically with anisotropic displacement parameters for all atoms. Due to the pronounced crystal mosaicity, a dynamic refinement was not feasible. The unit-cell parameters were verified by Rietveld refinement from powder X-ray diffraction data. The crystal structure was validated by many-body dispersion density functional theory (DFT) calculations. CuPcCl16 crystallizes in the space group C2/m (Z = 2), with the molecules arranged in layers. The structure agrees with that proposed in 1972.

Economic and mathematical approach to optimization of vacuum-freeze drying of the enzyme preparation inulinase Bacillus polymyxa 29

One of the promising directions of improving the processes of processing plant raw materials is bioconversion using enzyme preparations, the use of which allows you to significantly change, intensify and improve existing technologies for the production of food products as a system of energy-efficient processes. The subject of the study is the enzyme preparation of inulinase Bacillus polymyxa 29, which ensures the conversion of the plant polymer inulin to fructose. Fructose has an increased interest in food technologies as a safer human health alternative to sucrose. Fructose yield reaches 90–95%; the sweetness coefficient of fructose is 1.73 times higher than sucrose. Production of enzyme with maximum activity is achieved by vacuum-sublimation drying at time-programmed mode of heat supply control taking into account limitations due to quality of heat exchange and economic feasibility of the process. Method of selection of optimal solutions in vacuum-sublimation drying of feather preparation Bacillus polymyxa 29 according to profit index is proposed. The proposed approach resolved the main technical gap between productivity and energy consumption. An optimal loading of the sublimator has been established, which ensures the minimization of specific electric power consumption for various values of the initial moisture drying of the enzyme, taking into account the given efficiency of the vacuum sublimation dryer.

Hydrothermal SiO2 Nanopowders: Obtaining Them and Their Characteristics

The technological mode of obtaining amorphous SiO2 nanopowders based on hydrothermal solutions is proposed in this study. Polycondensation of orthosilicic acid as well as ultrafiltration membrane separation, and cryochemical vacuum sublimation were used. The characteristics of nanopowders were determined by tunneling electron microscopy, low-temperature nitrogen adsorption, X-ray diffraction, and small-angle X-ray scattering. The scheme allows to adjust density, particle diameters of nanopowders, specific surface area, as well as diameters, area and volume of the pore. Thus, the structure of nanopowders is regulated—the volume fraction of the packing of spherical particles in aggregates and agglomerates, the size of agglomerates, and the number of particles in agglomerates. The pour densities of the nanopowders depend on the SiO2 content in sols, which were 0.02 to 0.3 g/cm3. Nanoparticles specific surface area was brought to 500 m2/g by low temperature polycondensation. Nanoparticle aggregates specific pore volume (0.2–0.3 g/cm3) weakly depend on powders density. The volume fraction of the packing of SiO2 nanoparticles in aggregates was 0.6–0.7. Solid samples of compacted nanopowders had a compressive strength of up to 337 MPa. Possible applications of hydrothermal SiO2 nanopowders are considered.