High-Tech Material in a Salt Crust

Jülich researchers seek to reduce the cost of producing MAX phases and high-performance metals and ceramics using salt.

Jülich, 3 April 2019 – MAX phases are viewed as promising materials for the future, for example for turbines in power plants and aircraft, space applications, or medical implants. A new method developed by scientists from Forschungszentrum Jülich now makes it possible to produce this desirable material class on an industrial scale for the first time: a crust of salt protects the raw material from oxidation at a production temperature of more than 1,000 degrees Celsius – and can then simply be washed off with water. The method, which was recently published in the journal Nature Materials, can also be applied to other high-performance materials.

Verfahren ohne Vakuumtechnologie
Mit dem neuen Verfahren reicht nun schon ein normaler Ofen. Im Bild: Dr. Jesus Gonzalez-Julian (rechts) und Apurv Dash (links)
Forschungszentrum Jülich / Regine Panknin (click on the image to enlarge; image usage: please give credit for all images)

MAX phases unite the positive properties of both ceramics and metals. They are heat resistant and lightweight like ceramics, yet less brittle, and can be plastically deformed like metals. Furthermore, they are the material basis of MXenes, a largely unexplored class of compound that are similar to the “miracle material” graphene and have extraordinary electronic properties.

“In the past, there was no suitable method for producing MAX phases in powder form, which would be advantageous for further industrial processing. This is why MAX phases have not played any practical role in industrial application so far,” explains Junior Professor Dr. Jesus Gonzalez-Julian, young investigators group leader at Forschungszentrum Jülich.

The salt strategy

MAX phases are produced at temperatures higher than 1,000 degrees Celsius. At such high temperatures, the materials would normally react with atmospheric oxygen and oxidize, which is why they are usually produced in a vacuum or in a protective atmosphere of argon. The Jülich method is astonishingly simple by comparison: the researchers encapsulate the raw material with a salt – potassium bromide – which melts during the production process. A vacuum or argon atmosphere for additional protection is no longer needed.

Schema des Prozesses
Forschungszentrum Jülich / Apurv Dash

“A bath of molten salt thus protects the material and prevents it from coming in contact with atmospheric oxygen,” explains Apurv Dash, lead author of the study published in Nature Materials and doctoral researcher at Forschungszentrum Jülich.

At the same time, the salt acts as a separating agent: the components no longer bond together to form a compact solid, and allow the direct production of fine-grained powders. This is important because it avoids an additional long, energy- intensive milling process. As a positive side effect, the salt bath also reduces the synthesis temperature necessary to form the desired compound, which will additionally cut energy and production costs.

Salzkruste
Erstarrte Salzkruste nach dem Abkühlen
Forschungszentrum Jülich / Tobias Schlößer

With just salt and water

Methods using molten salt have been used for the powder production of non-oxide ceramics for some time. However, they require a protective argon atmosphere instead of atmospheric air, which increases both the complexity and production costs.

“Potassium bromide, the salt we use, is special because when pressurized, it becomes completely impermeable at room temperature. “We have now demonstrated that it is sufficient to encapsulate the raw materials tightly enough in a salt pellet to prevent contact with oxygen – even before the melting point of the salt is reached at 735 degrees Celsius. A protective atmosphere is thus no longer necessary,” explains Apurv Dash.

As with many scientific discoveries a little bit of luck played its part in inventing the method: vacuum furnaces are scarce because they are so expensive and they take a lot of effort to clean. To produce his powder, the Jülich doctoral researcher therefore resorted to testing a normal air furnace – successfully!

The new method is not limited to a certain material. The researchers have already produced a multitude of different MAX phases and other high-performance materials, such as titanium alloys for bioimplants and aircraft engineering. As a next step, the scientists are now planning to investigate industrial processes with which these powders can be processed further.

Video:

Falling Walls Lab 2018 - Apurv Dash - Breaking the Wall of Oxidation by Salting (Length: 2:30 min)

Images:

Dr. Jesus Gonzalez-Julian (links) und Apurv Dash (rechts)
Dr. Jesus Gonzalez-Julian (links) und Apurv Dash (rechts)
Forschungszentrum Jülich / Hiltrud Moitroux
MAX-Phase
MAX-Phasen vereinen Eigenschaften von Keramiken und Metallen
Forschungszentrum Jülich / Tobias Schlößer
Materialherstellung im Salzmantel
Materialherstellung im Salzmantel: dichtes (links) und poröses (rechts) Titan
Forschungszentrum Jülich / Hiltrud Moitroux

Original publication:

Molten salt shielded synthesis of oxidation prone materials in air
Apurv Dash, Robert Vaßen, Olivier Guillon, Jesus Gonzalez-Julian
Nature Materials (published 1 April 2019), DOI: 10.1038/s41563-019-0328-1

Further information:

Institute of Energy and Climate Research – Materials Synthesis and Processing (IEK-1)

Ceramic Matrix Composites

Young investigators group “Ceramic Matrix Composites”

This work was funded by Germany’s Federal Ministry of Education and Research (Bundesministerium für Bildung und Forschung) under the MAXCOM project (03SF0534).

Download press release:

Press release (pdf / 76 KB)

Contact:

Prof. Dr. Olivier Guillon
Head of the Institute of Energy and Climate Research – Materials Synthesis and Processing (IEK-1)
Tel.: +49 2461 61-5181
Email: o.guillon@fz-juelich.de

Prof. Dr. Robert Vaßen
Deputy director and department head at the Institute of Energy and Climate Research – Materials Synthesis and Processing (IEK-1)
Tel: +49 2461 61-6108
Email: r.vassen@fz-juelich.de

Dr. Jesus Gonzalez-Julian
Junior Professor and team leader at the Institute of Energy and Climate Research – Materials Synthesis and Processing (IEK-1)
Tel: +49 2461 61-96761
Email: j.gonzalez@fz-juelich.de

Apurv Dash
Doctoral researcher at the Institute of Energy and Climate Research –
Materials Synthesis and Processing (IEK-1)
Tel: +49 2461 61-4421
Email: a.dash@fz-juelich.de

Press contact:

Tobias Schlößer
Press officer, Corporate Communications
Tel: +49 2461 61-4771
Email: t.schloesser@fz-juelich.de

Last Modified: 29.10.2022