Laboratory 3D micro X-ray diffraction

Project Information

LabmyXRD

Grant agreement ID: 101069404

DOI

10.3030/101069404

Project closed

EC signature date 15 March 2022

Start date 1 May 2022

End date 31 October 2023

Funded under

• European Research Council (ERC)

Total cost

No data

EU contribution

€ 150 000,00

Coordinated by

DANMARKS TEKNISKE UNIVERSITET
Denmark

Periodic Reporting for period 1 - LabmyXRD (Laboratory 3D micro X-ray diffraction)

Reporting period: 2022-05-01 to 2023-10-31

Summary of the context and overall objectives of the project

When characterizing a three-dimensional (3D) structure using two-dimensional (2D) experimental tools, great care has to be taken not to get a false impression of the reality. This is critical when characterizing crystalline materials: whereas essentially all materials’ microstructures are 3D, the by far most widely applied microstructural characterization tool is microscopy, which provides 2D images only.

Motivated by the need for much more comprehensive 3D data, intense efforts were devoted in the early 2000’ies to the development of synchrotron X-ray based 3D characterization tools, and today a palette of X-ray orientation imaging methods is available at the large international synchrotron facilities. However, characterization tools at synchrotron sources are insufficient: availability of beam time there is very limited, extended measurement times (> 1 week) are not realistic, and the turnaround time (from idea to result) is typically a year or more. Similar tools working in the home-laboratories are required to realize the dream of making 3D characterization the new golden standard.

Today only one laboratory X-ray tool exists for a crystallographic orientation mapping (LabDCT). LabDCT can image grains larger than 20 μm, and the grains have to be defect-free.

Our solution to overcome these limitations is to develop a laboratory-based 3D micro X-ray Laue diffraction (LabμXRD) technique using newly developed and commercially available X-ray optics to focus the X-ray beam from a laboratory X-ray instrument, and then adapt scanning and translation principles.

The technical objectives are:
• to build and optimize LabμXRD set-ups using both open-architectural and commercial systems,
• to validate and benchmark the spatial resolution by other methods wherever possible,
• to develop measurement and analysis methodologies matching industrial needs.

The commercial objectives are:
• to thoroughly map the market and the competitive landscape, incl. talking to end users,
• to complete a first business plan,
• to work with instrument suppliers to get commitment to commercialize the technology.

End users are scientists and industrial researchers/developers alike, who need microstructural and crystallographic orientation characterization of crystalline samples or components. Today these end users mainly use electron microscopy, LabDCT and/or synchrotron methods for their characterization.

If LabμXRD can be manufactured to the specification, and commercialized at a reasonable sales price, we foresee that it will in time supplement or even replace LabDCT. In the longer perspective (within the order of 10 years) we foresee LabμXRD to also replace at least a part of the electron back scattering diffraction market, and become the new golden standard for microstructural characterization.

Work performed from the beginning of the project to the end of the period covered by the report and main results achieved so far

The LabμXRD idea was originated and patented (patent application filed in July 2020 (WO2022013127A1)) in the ERC Advanced Grant M4D led by the present PI. The main activities performed in this accompanying ERC POC project include:

• Detailed characterization of the commercially acquired X-ray focusing optics, in an in-house open-architectural X-ray set-up. Slight optimization of the optics was needed, and successfully performed.

• Test of the basic idea of LabμXRD both in the in-house open-architectural X-ray set-up and in a commercial X-ray system (Zeiss Versa). Whereas the LabμXRD principles were documented to be feasible, issues related to manual alignment of the optics and very long measurement times were identified. The alignment issue was easily overcome by purchasing an automated stage. As the LabμXRD principle requires sample scanning, an automatic sample stage was also purchased and successfully implemented. Finally, we could document that if a photon counting detector was used, the recording time per diffraction image could be reduced from tens of minutes to a few seconds. This is of utmost importance, as the measuring time of a complete 3D microstructure map will thus be in the order of hours instead of days, making LabμXRD a feasible tool also for industrial investigations.

• Samples appropriate for documenting the spatial resolution of LabμXRD, which can be validated by other methodologies than LabμXRD, had to be found. We have assembled a series of samples including metallic powders (LabμXRD results validated by absorption contrast X-ray tomography), commercially available micron size single crystals (LabμXRD results validated by electron microscopy) and fine grained metallic samples (LabμXRD results validated by synchrotron X-ray measurements).

• Software had to be developed to index the obtained X-ray data - i.e. software that uses the diffracted signal as input and can map the crystallographic orientations in 3D. Two software systems were developed, one based on the commercial LabDCT software and one totally in-house developed system based on a dictionary-approach. In the longer run, the first one is the more likely candidate to be further developed.

The significant achievement of this ERC POC project is that the concept of LabμXRD has been proven and its innovation potential has been demonstrated by visualising grains with sizes down to 5 μm in a metal sample using a setup with a conventional X-ray source, off-the-shelf X-ray optics, and a state-of-the-art X-ray detector.

Progress beyond the state of the art and expected potential impact (including the socio-economic impact and the wider societal implications of the project so far)

Given the society's rising demand for novel and more efficient materials, there is a growing interest in characterization methods that can provide detailed analysis and insights into the properties of these materials. Here LabμXRD will become a unique tool. It potential impact can hardly be overstated, as it will enable 3D characterization at the right length scales in home-laboratories.

We evaluate the LabμXRD technology to be on TRL3 now, and have submitted a Horizon-EIC-2023-Transitionopen-01 application, in which we, together with partners, expect to advance LabμXRD from TRL3 to TRL6. The next steps will include design and development of a prototype version of LabμXRD, and demonstrating the novel technology on next-generation materials.

We have the patent application (WO2022013127A1 Laboratory-based 3D scanning X-ray scanning Laue micro-diffraction system and method) for the LabμXRD technology, and a PCT application was subsequently filed in July 2021. During this ERC POC project, we negotiated a license agreement with the Danish company Xnovo Technology ApS, who now has an exclusive license to this IP. If we can secure the necessary funding for the further development together with Xnovo (and possibly also with other partners), we do not expect any roadblocks for the commercial exploitation of the technology, which Xnovo also foresees to have a remarkable business opportunity.

The main results of this ERC POC project are thus that the LabμXRD concept is proven, the innovation potential is documented, a license agreement is signed with the by far most relevant commercial company (Xnovo Technology ApS), plans for a prototype version are conceived in collaboration with Xnovo, and an application for funding of the further exploitation endeavor of LabμXRD has been submitted.