Slug Flow Coprecipitation Synthesis of Uniformly-Sized Oxalate Precursor Microparticles for Improved Reproducibility and Tap Density of Li(Ni0.8Co0.1Mn0.1)O2 Cathode Materials.

The microparticle quality and reproducibility of Li(Ni0.8Co0.1Mn0.1)O2 (NCM811) cathode materials are important for Li-ion battery performance but can be challenging to control directly from synthesis. Here, a scalable reproducible synthesis process is designed based on slug flow to rapidly generate uniform micron-size spherical-shape NCM oxalate precursor microparticles at 25-34 °C. The whole process takes only 10 min, from solution mixing to precursor microparticle generation, without needing aging that typically takes hours. These oxalate precursors are convertible to spherical-shape NCM811 oxide microparticles, through a preliminary design of low heating rates (e.g., 0.1 and 0.8 °C/min) for calcination and lithiation. The outcome oxide cathode particles also demonstrate improved tap density (e.g., 2.4 g mL-1 for NCM811) and good specific capacity (202 mAh g-1 at 0.1 C) in coin cells and reasonably good cycling performance with LiF coating.

Scalable Advanced Li(Ni0.8Co0.1Mn0.1)O2 Cathode Materials from a Slug Flow Continuous Process.

Li[Ni0.8Co0.1Mn0.1]O2 (LNCMO811) is the most studied cathode material for next-generation lithium-ion batteries with high energy density. However, available synthesis methods are time-consuming and complex, restricting their mass production. A scalable manufacturing process for producing NCM811 hydroxide precursors is vital for commercialization of the material. In this work, a three-phase slug flow reactor, which has been demonstrated for its ease of scale-up, better synthetic control, and excellent uniform mixing, was developed to control the initial stage of the coprecipitation of NCM811 hydroxide. Furthermore, an equilibrium model was established to predict the yield and composition of the final product. The homogeneous slurry from the slug flow system was obtained and then transferred into a ripening vessel for the necessary ripening process. Finally, the lithium-nickel-cobalt-manganese oxide was obtained through the calcination of the slug flow-derived precursor with lithium hydroxide, having a tap density of 1.3 g cm-3 with a well-layered structure. As-synthesized LNCMO811 shows a high specific capacity of 169.5 mAh g-1 at a current rate of 0.1C and a long cycling stability of 1000 cycling with good capacity retention. This demonstration provides a pathway toward scaling up the cathode synthesis process for large-scale battery applications.

Recrystallization of Adenosine for Localized Drug Delivery.

Adenosine (ADO) is an endogenous metabolite with immense potential to be repurposed as an immunomodulatory therapeutic, as preclinical studies have demonstrated in models of epilepsy, acute respiratory distress syndrome, and traumatic brain injury, among others. The currently licensed products Adenocard and Adenoscan are formulated at 3 mg/mL of ADO for rapid bolus intravenous injection, but the systemic administration of the saline formulations for anti-inflammatory purposes is limited by the nucleoside's profound hemodynamic effects. Moreover, concentrations that can be attained in the airway or the brain through direct instillation or injection are limited by the volumes that can be accommodated in the anatomical space (<5 mL in humans) and the rapid elimination by enzymatic and transport mechanisms in the interstitium (half-life <5 s). As such, highly concentrated formulations of ADO are needed to attain pharmacologically relevant concentrations at sites of tissue injury. Herein, we report a previously uncharacterized crystalline form of ADO (rcADO) in which 6.7 mg/mL of the nucleoside is suspended in water. Importantly, the crystallinity is not diminished in a protein-rich environment, as evidenced by resuspending the crystals in albumin (15% w/v). To the best of our knowledge, this is the first report of crystalline ADO generated using a facile and organic solvent-free method aimed at localized drug delivery. The crystalline suspension may be suitable for developing ADO into injectable formulations for attaining high concentrations of the endogenous nucleoside in inflammatory locales.

The Loading of Luminescent Magnetic Nanocomposites Fe3O4@Polyaniline/Carbon Dots for Methotrexate and Its Release Behavior In Vitro.

In the present study we developed novel luminescent magnetic nanocomposites termed Fe3O4@polyaniline/carbon dots. First, Fe3O4 magnetic nanoparticles were prepared by the coprecipitation method. The nanoparticles were then coated with polyaniline using the in situ growth method to form Fe3O4@polyaniline nanohybrids, which were endowed with amino functional groups on the surface and avoided the aggregation of Fe3O4 nanoparticles. The X-ray diffraction pattern demonstrated that the crystalline phase of the Fe3O4 nanoparticles was an inverse spinel structure and was not changed in the Fe3O4@polyaniline nanohybrids. The saturation magnetization and the coercive force of the as-prepared Fe3O4@polyaniline nanohybrids measured by a vibrating sample magnetizer were 63.7 emu·g-1 and zero respectively, which indicated that the Fe3O4@polyaniline nanohybrids exhibited excellent superparamagnetism. The Fe3O4@polyaniline nanohybrids were conjugated with carbon dots, prepared from orange juice, via the amide bond between the amino groups on the surface of the Fe3O4@polyaniline nanohybrids and the carboxyl groups on the surface of carbon dots. The obtained luminescent magnetic nanocomposites Fe3O4@polyaniline/carbon dots showed good photoluminescent properties, which hinted that the nanocomposites have potential in drug tracing and magnetic targeted drug delivery. Finally, the anticancer drug methotrexate was loaded into the Fe3O4@polyaniline/carbon dots nanocomposites, forming a novel magnetic targeted drug delivery system. The results confirmed that the novel drug delivery system exhibited excellent drug-loading capability for methotrexate of ca. 70%, and emits strong fluorescence at the wavelength of 360 nm. An in vitro release experiment of the drug delivery system indicated that the cumulative release percentage of methotrexate was 17.2% in the phosphate-buffered saline (pH = 7.4) within 36 h.

Aggregation-induced emission properties of hydrothermally synthesized Cu-In-S quantum dots.

Novel Cu-In-S quantum dots (CIS QDs), which exhibit interesting aggregation-induced emission (AIE) properties, were successfully prepared via a hydrothermal method. When the solvent was changed from water to 90 vol% DMSO, the photoluminescence intensity of the as-prepared CIS QDs was enhanced about 126-fold.