Ball size or ball mass – what matters in organic mechanochemical synthesis?

Michalchuk, Adam A. L.; Tumanov, Ivan A.; Boldyreva, Elena V.

doi:10.1039/c8ce02109k

Cited by 55 publications

(72 citation statements)

References 43 publications

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“…The presented results further our understanding of fundamental principles and mechanisms of mechanochemistry, an area that has recently attracted signicant interest. [32][33][34][35][36][37][38][39][40][41][42] While chemical autocatalysis is not the only potential reason for appearance of sigmoidal kinetics in a mechanochemical reaction, ‡ this study provides direct evidence that such a model is relevant for mechanochemical reactions and, in principle, may be broadly applicable to water-forming acid-base milling reactions. The enhancement of mechanochemical reactions in liquid-assisted grinding can sometimes be explained by a purely physical effects of dissolution and having a liquid phase present.…”

mentioning

confidence: 75%

In situ monitoring of mechanochemical synthesis of calcium urea phosphate fertilizer cocrystal reveals highly effective water-based autocatalysis

et al. 2020

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confidence: 75%

In situ monitoring of mechanochemical synthesis of calcium urea phosphate fertilizer cocrystal reveals highly effective water-based autocatalysis

et al. 2020

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“…Mechanochemical reactions are indeed far from trivial, as they involve both physical steps (mixing of reagents, particle size reduction, creation of reactive surfaces, diffusion of atoms/molecules at the interfaces…) and chemical steps (chemical reactions), both of which are important for the system to evolve towards a given product. [53][54] Despite numerous investigations, some of which include in situ measurements and/or innovative designs of the milling equipment, [54][55][56][57][58][59] many blind spots remain regarding both the physics and chemistry of mechanochemical reactions. This is even more true when common techniques like X-ray diffraction are not informative, as observed here for the four p-and d-block oxides, as well as for the mixed SiO 2 /TiO 2 system.…”

Section: Atomic-level Insight Into Reactions Occurring During Ball-mimentioning

confidence: 99%

Direct 17O-Isotopic Labeling of Oxides Using Mechanochemistry

Chen¹,

Gaillard²,

Mentink-Vigier³

et al. 2019

Preprint

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While oxygen-17 NMR is increasingly being used for elucidating the structure and reactivity of complex molecular and materials systems, much effort is still required for it to become a routine analytical technique. One of the main difficulties for its development comes from the very low natural abundance of oxygen-17, which implies that isotopic labeling is generally needed prior to NMR analyses. However, 17O-enrichment protocols are often unattractive in terms of cost, safety, and/or practicality, even for compounds as simple as metal oxides. Here, we demonstrate how mechanochemistry can be used in a highly efficient way for the direct 17O-isotopic labeling of a variety of s-, p- and d-block oxides which are of major interest for the preparation of functional ceramics and glasses: Li2O, CaO, Al2O3, SiO2, TiO2, and ZrO2. For each oxide, the enrichment step was performed under ambient conditions in less than 1 hour and at low cost, which makes these synthetic approaches highly appealing in comparison to the existing literature. Using high-resolution 17O solid state NMR and Dynamic Nuclear Polarization, atomic-level insight into the enrichment process is achieved, especially for titania and alumina. Indeed, it was possible to demonstrate that enriched oxygen sites are present not only at the surface, but also within the oxide particles. Moreover, information on the actual reactions occurring during the milling step could be obtained by 17O NMR, both in terms of their kinetics and the nature of the reactive species. Finally, it was demonstrated how high resolution 17O NMR can be used for studying the reactivity at the interfaces between different oxide particles during ball-milling, especially in cases when X-ray diffraction techniques are uninformative. More generally, such investigations will be useful not only for producing 17O-enriched precursors efficiently, but also for understanding better mechanisms of mechanochemical processes themselves. <br>

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“…Increasing the weight of milling media in experiment B corresponds to an increase in energy delivered to the reaction system, and is anticipated to lead to an increase in reaction rate. 32 Such an increase was indeed observed, along with the transient appearance of Form II of the (nic)$(adi) cocrystal. Forms I and II appeared concomitantly and their content increased almost simultaneously, indicating the conversion of the intermediate (nic) 2 $(adi) via two competing pathways.…”

Section: In Situ X-ray Powder Diffractionmentioning

confidence: 77%

“…23c Whereas such thermodynamic considerations may suggest a route to predict the course of mechanochemical reactions, 12b,23d it remains unclear whether mechanochemical reactions of organic and metal-organic materials generally conform to Ostwald's rule of stages. While it is well established that milling frequency, [24][25][26] reaction jar lling, 26,27a,28 size or mass of milling media 26,27b, [30][31][32] all affect rates of product formation, there are only a handful of reports discussing the inuence of energy input, 26,27,31,33,34 mixing properties, or design of the milling assembly in organic mechanochemistry. 26,31,[34][35][36][37] In fact, the latter appears to have remained unexplored in the context of polymorphism in mechanochemical reactions.…”

Section: Introductionmentioning

confidence: 99%