Swiss Light Source, Paul Scherrer Institut , 5232 Villigen PSI, Switzerland.
Laboratory of Crystallography, DQMP, University of Geneva , quai Ernest-Ansermet 24, 1211 Geneva, Switzerland.
Anal Chem. 2017 Dec 19;89(24):13176-13181. doi: 10.1021/acs.analchem.7b02871. Epub 2017 Dec 1.
The renewed interest of mechanochemistry as an ecofriendly synthetic route has inspired original methodologies to probe reactions, with the aim to rationalize unknown mechanisms. Recently, Friščić et al. ( Nat. Chem. 2013 , 5 , 66 - 73 , DOI: 10.1038/nchem.1505 ) monitored the progress of milling reactions by synchrotron X-ray powder diffraction (XRPD). For the first time, it was possible to acquire directly information during a mechanochemical process. This new methodology is still in its early stages, and its development will definitively transform the fundamental understanding of mechanochemistry. A new type of in situ ball mill setup has been developed at the Materials Science beamline (Swiss Light Source, Paul Scherrer Institute, Switzerland). Its particular geometry, described here in detail, results in XRPD data displaying significantly lower background and much sharper Bragg peaks, which in turn allow more sophisticated analysis of mechanochemical processes, extending the limits of the technique.
作为一种环保型合成途径，机械化学的重新兴起激发了人们探索反应的原创方法，旨在推理未知的反应机制。最近，Friščić 等人（Nat. Chem. 2013, 5, 66-73, DOI: 10.1038/nchem.1505）通过同步加速器 X 射线粉末衍射（XRPD）监测研磨反应的进展。这是首次可以在机械化学过程中直接获取信息。这种新方法仍处于早期阶段，其发展必将改变人们对机械化学的基本认识。在材料科学光束线（瑞士光源，保罗谢勒研究所，瑞士）开发了一种新型的原位球磨机装置。其特殊的几何形状，在这里详细描述，导致 XRPD 数据显示出明显更低的背景和更尖锐的布拉格峰，这反过来又允许对机械化学过程进行更复杂的分析，从而扩展了该技术的极限。
