Hydrothermal synthesis is a chemical process that has gained much interest in recent years, especially for the synthesis of LiFePO4 since it is a method that requires a relatively low temperature, short reaction time, and it is reproducible. In this work, LiFePO4 microparticles have been synthesized by means of a fast heating system (sand bath) under hydrothermal conditions. The experiments have been carried out under two different heating rates (86 °C/min and 5.26 °C/min), two different residence times (5 and 30 min), and two different cooling rates (−455 °C/min and −8 °C/min). The effects that these three parameters had on the synthesized particles were verified using several techniques such as X-ray diffraction and scanning electron microscopy. It was observed that the heating rate had a great influence on the purity, crystallization, and morphology of the synthesized LiFePO4 particles. In addition, the high influence of cooling rate on the crystallization and morphology of the particles was also analyzed.

The use of micro- and nanoparticles is gaining more and more importance because of their wide range of uses and benefits based on their unique mechanical, physical, electrical, optical, electronic, and magnetic properties. In recent decades, supercritical fluid technologies have strongly emerged as an effective alternative to other numerous particle generation processes, mainly thanks to the peculiar properties exhibited by supercritical fluids. Carbon dioxide and water have so far been two of the most commonly used fluids for particle generation, the former being the fluid par excellence in this field, mainly, because it offers the possibility of precipitating thermolabile particles. Nevertheless, the use of high-pressure and -temperature water opens an innovative and very interesting field of study, especially with regards to the precipitation of particles that could hardly be precipitated when CO2 is used, such as metal particles with a considerable value in the market. This review describes an innovative method to obtain micro- and nanoparticles: hydrothermal synthesis by means of near and supercritical water. It also describes the differences between this method and other conventional procedures, the most currently active research centers, the types of particles synthesized, the techniques to evaluate the products obtained, the main operating parameters, the types of reactors, and amongst them, the most significant and the most frequently used, the scaling-up studies under progress, and the milestones to be reached in the coming years.

Lithium-ion batteries (LIBs) have gained much interest in recent years because of the increasing energy demand and the relentless progression of climate change. About 30% of the manufacturing cost for LIBs is spent on cathode materials, and its level of development is lower than the negative electrode, separator diaphragm and electrolyte, therefore becoming the “controlling step”. Numerous cathodic materials have been employed, LiFePO4 being the most relevant one mainly because of its excellent performance, as well as its rated capacity (170 mA·h·g−1) and practical operating voltage (3.5 V vs. Li+/Li). Nevertheless, producing micro and nanoparticles with high purity levels, avoiding the formation of iron oxides, and reducing the operating cost are still some of the aspects still to be improved. In this work, we have applied two heating rates (slow and fast) to the same hydrothermal synthesis process with the main objective of obtaining, without any reducing agents, the purest possible LiFePO4 in the shortest time and with the lowest proportion of magnetite impurities. The reagents initially used were: FeSO4, H3PO4, and LiOH, and a crucial phenomenon has been observed in the temperature range between 130 and 150 °C, being verified with various techniques such as XRD and SEM.