3-D-printed jars in ball-milling experiments

June 27, 2017, International Union of Crystallography
Thin-walled jar with a groove; isometric view with a cut (left) and cross section (right). Credit: Tumanov et al

Mechanochemistry is a widespread synthesis technique in all areas of chemistry. Various materials have been synthesized by this technique when the classical wet chemistry route is not satisfactory. Characterization of the reaction mixture is however much less accessible than in solutions.

Recently, in situ observations of mechanochemical reactions have been achieved by X-ray and Raman spectroscopy. Solid-state reactions can be directly tracked, revealing phase transitions and other material transformations during synthesis in a ball mill jar. This has become increasingly popular in different fields of mechanochemistry.

As the X-rays go through the entire jar, the present a high background due to the scattering from the thick walls of the jar. Also, broad diffraction peaks are expected from the sample as a result of probing a large sample area covering the entire jar. An extra complexity arises from diffraction on the milling balls.

Tumanov et al. reasoned that these issues can be resolved by modifying the geometry and material of the milling jar. But, making a jar with a complex geometry using traditional production techniques is complicated, especially at the stage of creating a prototype, when introducing changes into a design should be facile. For this reason they decided to use a 3D printer for the purpose. They show how this useful production tool can quickly make milling jars optimized for improved background, absorption and angular resolution in X-ray powder diffraction experiments; the jars are also more resistant to solvents compared with standard acrylic jars. 3D printing allows for low-cost fast production on demand.

Source files for printing the jars are available as supporting information for the paper.

Explore further: Video: Mechanisms of mechanochemistry

More information: Nikolay Tumanov et al, 3D-printed jars for ball-milling experiments monitored in situ by X-ray powder diffraction, Journal of Applied Crystallography (2017). DOI: 10.1107/S1600576717006744

Related Stories

Video: Mechanisms of mechanochemistry

August 20, 2015

The solvent-free mechanochemical synthesis of a metal-organic framework, ZIF-8, was followed in real-time by in situ X-ray diffraction monitoring. Formation of the open framework is recognized by the appearance of new diffraction ...

Researchers create perovskites via mechanochemistry

January 15, 2016

Perovskites, substances that perfectly absorb light, are the future of solar energy. Now, a rapid and environmentally safe method of production has been developed by chemists from Warsaw, Poland. Perovskites can now be synthesized ...

Recommended for you

World's oldest cheese found in Egyptian tomb

August 15, 2018

Aging usually improves the flavor of cheese, but that's not why some very old cheese discovered in an Egyptian tomb is drawing attention. Instead, it's thought to be the most ancient solid cheese ever found, according to ...

Molecular switch detects metals in the environment

August 15, 2018

An international team led by researchers from the University of Geneva (UNIGE), Switzerland, has designed a family of molecules capable of binding to metal ions present in the surrounding environment and providing an easily ...

A near-infrared fluorescent dye for long term bioimaging

August 15, 2018

A group of chemists at the Institute of Transformative Bio-Molecules (ITbM), Nagoya University, has developed a new near infrared (NIR) emitting photostable fluorescent dye PREX 710 (photo-resistant xanthene dye which can ...

Lipid droplets play crucial roles beyond fat storage

August 14, 2018

Lipid droplets: they were long thought of merely as the formless blobs of fat out of which spare tires and muffin tops were made. But these days, they're "a really hot area of research," says Michael Welte, professor and ...

0 comments

Please sign in to add a comment. Registration is free, and takes less than a minute. Read more

Click here to reset your password.
Sign in to get notified via email when new comments are made.