3D printed devices and infrastructure for liquid sample delivery at the European XFEL.

Mohammad Vakili,Katerina Dörner,Elisa Delmas,Huijong Han,Marco Kloos,Grant Mills,Frederico A Lima,Simon Dold,Adam Round,Richard Bean,Florian Otte,Johan Bielecki,Robin Schubert,Romain Letrun,Joachim Schulz,Adrian P Mancuso,Yoonhee Kim,Michaël Heymann ,Joana Valério ,J Knoška ,Raphaël De Wijn

doi:10.1107/s1600577521013370

Mohammad Vakili, Katerina Dörner + Show 19 more

Open Access

https://doi.org/10.1107/s1600577521013370

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Abstract

The Sample Environment and Characterization (SEC) group of the European X-ray Free-Electron Laser (EuXFEL) develops sample delivery systems for the various scientific instruments, including systems for the injection of liquid samples that enable serial femtosecond X-ray crystallography (SFX) and single-particle imaging (SPI) experiments, among others. For rapid prototyping of various device types and materials, sub-micrometre precision 3D printers are used to address the specific experimental conditions of SFX and SPI by providing a large number of devices with reliable performance. This work presents the current pool of 3D printed liquid sample delivery devices, based on the two-photon polymerization (2PP) technique. These devices encompass gas dynamic virtual nozzles (GDVNs), mixing-GDVNs, high-viscosity extruders (HVEs) and electrospray conical capillary tips (CCTs) with highly reproducible geometric features that are suitable for time-resolved SFX and SPI experiments at XFEL facilities. Liquid sample injection setups and infrastructure on the Single Particles, Clusters, and Biomolecules and Serial Femtosecond Crystallography (SPB/SFX) instrument are described, this being the instrument which is designated for biological structure determination at the EuXFEL.

Highlights

This work presents the current pool of 3D printed liquid sample delivery devices, based on the two-photon polymerization (2PP) technique. These devices encompass gas dynamic virtual nozzles (GDVNs), mixing-GDVNs, high-viscosity extruders (HVEs) and electrospray conical capillary tips (CCTs) with highly reproducible geometric features that are suitable for time-resolved serial femtosecond X-ray crystallography (SFX) and singleparticle imaging (SPI) experiments at X-ray free-electron lasers (XFELs) facilities
The velocities of the liquid jets generated by 2PP-3D printed GDVNs were determined by two experimental methods in high vacuum
In the first method (‘droplet PIV’), the droplets formed after jet break up are exposed twice in the same camera image by two consecutive nanosecond laser pulses separated in time by a delay Át (Grunbein, Shoeman et al, 2018)

Summary

Introduction

Typically a few tens of femtoseconds long, an XFEL can provide the order of magnitude of photons that a synchrotron delivers in a second This places stringent requirements on the XFEL sample delivery that the Sample Environment and Characterization (SEC) group of the European X-ray Free-Electron Laser (EuXFEL) provides to its users. One imaging method in particular, serial femtosecond X-ray crystallography (SFX), benefits from the short pulses and high photon flux of an XFEL to outrun the radiation damage of crystals that would limit the resolution in conventional technologies (Schlichting, 2015). This diffractionbefore-destruction approach makes use of the fact that radiation damage takes time to manifest after X-ray excitation. This method may be used for structure determination without the need to crystalize at all (Neutze et al, 2000; Seibert et al, 2011; Bielecki et al, 2020)

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