Skip to main page content
U.S. flag

An official website of the United States government

Dot gov

The .gov means it’s official.
Federal government websites often end in .gov or .mil. Before sharing sensitive information, make sure you’re on a federal government site.

Https

The site is secure.
The https:// ensures that you are connecting to the official website and that any information you provide is encrypted and transmitted securely.

Access keys NCBI Homepage MyNCBI Homepage Main Content Main Navigation
. 2022 Mar 1;29(Pt 2):331-346.
doi: 10.1107/S1600577521013370. Epub 2022 Feb 15.

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

Mohammad Vakili  1 , Johan Bielecki  1 , Juraj Knoška  2 , Florian Otte  1 , Huijong Han  1 , Marco Kloos  1 , Robin Schubert  1 , Elisa Delmas  1 , Grant Mills  1 , Raphael de Wijn  1 , Romain Letrun  1 , Simon Dold  1 , Richard Bean  1 , Adam Round  1 , Yoonhee Kim  1 , Frederico A Lima  1 , Katerina Dörner  1 , Joana Valerio  1 , Michael Heymann  3 , Adrian P Mancuso  1 , Joachim Schulz  1
Affiliations

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

Mohammad Vakili et al. J Synchrotron Radiat. .

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.

Keywords: FEL physics; X-ray scattering; aerosols; crystallography; high-viscosity extrusion; instrumentation; liquid jets; microfluidics; rapid mixing; sample delivery; single-particle imaging.

PubMed Disclaimer

Figures

Figure 1
Figure 1
The high repetition rate X-ray pulse pattern at the EuXFEL. X-ray pulses arrive in 10 Hz trains at the sample and each train can provide up to 2700 ultrashort pulses.
Figure 2
Figure 2
(a) An overview of the 2PP-3D printed mix-and-inject device (i.e. mixing-GDVN) consisting of a micromixer, a GDVN (type C) and a connective capillary in between. The capillary extension was chosen to be L 2 = 28 mm. (b) A microscopy image showing lysozyme crystal delivery on the SPB/SFX instrument (10× magnification, NA 0.28, pixel size ∼0.65 µm). Upstream from the depicted X-ray interaction region, the crystals enter from the main channel of the mixing device at 7 µl min−1 and are flow-focused by pure water entering from the side channel at 70 µl min−1. Downstream, the 11-fold diluted sample then enters the GDVN (type C, 100 µm liquid orifice). With a helium pressure of 550 psi (Q g = 34 mg min−1), a liquid jet of 7.5 µm in diameter delivers the crystals into the X-ray focus. With our prediction formula [Fig. 4(b)], the jet velocity was determined to be 30.5 m s−1. (c) A microscopy image of the lysozyme crystal dispersion from the utilized sample reservoir showing the near-monodisperse microcrystals. (d) A background-corrected detector image of lysozyme diffraction from the same 11-fold dilution collected on the AGIPD 1M detector. The detector (pixel size is 200 µm × 200 µm) consists of four movable quadrants, each quadrant consisting of four static independent modules. Each module is 26 mm × 103 mm (128 × 512 pixels) large and consists of 2 × 8 ASICs (application-specific integrated circuits). The magnified region (green rectangle) shows Bragg reflections within 2 × 2 ASICs.
Figure 3
Figure 3
Side view images (10× magnification, NA 0.28, 1075 × 310 pixels2 detection area, pixel size ∼0.65 µm) taken inside the SPB/SFX sample chamber, each depicting a thin liquid jet (water) generated by a 75–60–75 (µm) GDVN using a liquid flow rate of Q l = 10 µl min−1 and an applied gas pressure of p He = 400 psi (Q g = 25 mg min−1). (a) The liquid jet in the absence of X-rays. (b) X-ray pulses arrive at f = 0.564 MHz (with 30 pulses per train) and create gaps in the liquid column (gap-to-gap spacing Δx = 104.7 µm). The X-ray interaction with the jet hence reveals a jet velocity of v jet = Δx × f pulse = 59.1 m s−1. (c) Two optical lasers (λ = 532 nm), each with a 5 ns pulse duration, illuminate the droplets 2 mm downstream of the jet region. The delay time between the two laser pulses is 119 ns and reveals a droplet displacement of Δx = 7.2 µm. Therefore, dual-pulse laser illumination reveals a droplet velocity of v droplet = Δx/Δt opt.pulse = 60.1 m s−1. The determined jet velocities imply a jet diameter of d jet = [4Q l/(πv)]1/2 ≃ 2 µm.
Figure 4
Figure 4
(a, b) Plots of the experimentally determined jet velocities for the four different GDVN types as a function of applied liquid and gas flow rates. Circles represent data from the jet explosion method, while stars denote velocities from the droplet PIV method. In panel (b) the broken line describes the jet velocity prediction formula v jet = a + b × (Q g/D g 2)1/2/(Q l)1/4, where the constants have the numerical values a = 8.35 and b = 1022 if Q g is given in mg min−1, D g in µm, Q l in µl min−1 and v jet in m s−1. (c) The corresponding jet diameters are calculated via d jet = [4Q l/(πv)]1/2.
Figure 5
Figure 5
(a) A photograph of an assembled micromixer (type Y with 100 µm ID) before connection to a GDVN. (b) A microscopic image showing a detailed view of the mixing initiation area. (c) Magnified regions of the mixing channel–capillary interface, showing the 3D hydrodynamic flow focusing of a central ink stream (main channel) where the diluting water (entering from the side channel) runs at various flow rates. The mixed species is seamlessly transferred from the 2PP-3D printed part into the capillary extension.
Figure 6
Figure 6
(a) Droplet diameters achieved as a function of applied liquid flow rate Q for different conductivities K. (b) In the dimensionless parametrization of the flow rate and droplet (Maißer et al., 2013 ▸), the droplet diameters from the different conductivities fall on the same curve. (c) A side-view microscopy image (0.92 µm pixel size) of the 2PP-3D printed CCT. The 40 µm ID of the electrospray tip exactly matches the ID of the utilized fused silica capillary and the 30° angle at the tip is seamlessly transferred to the angle of the formed liquid cone. The tip–liquid interface is indicated with the dotted red line.
See this image and copyright information in PMC

Similar articles

See all similar articles

Cited by

See all "Cited by" articles

References

    1. Allahgholi, A., Becker, J., Delfs, A., Dinapoli, R., Goettlicher, P., Greiffenberg, D., Henrich, B., Hirsemann, H., Kuhn, M., Klanner, R., Klyuev, A., Krueger, H., Lange, S., Laurus, T., Marras, A., Mezza, D., Mozzanica, A., Niemann, M., Poehlsen, J., Schwandt, J., Sheviakov, I., Shi, X., Smoljanin, S., Steffen, L., Sztuk-Dambietz, J., Trunk, U., Xia, Q., Zeribi, M., Zhang, J., Zimmer, M., Schmitt, B. & Graafsma, H. (2019). J. Synchrotron Rad. 26, 74–82. - PMC - PubMed
    1. Bean, R. J., Aquila, A., Samoylova, L. & Mancuso, A. P. (2016). J. Opt. 18, 074011.
    1. Bernardeschi, I., Ilyas, M. & Beccai, L. (2021). Adv. Intell. Syst. 3, 2100051.
    1. Beyerlein, K. R., Adriano, L., Heymann, M., Kirian, R., Knoška, J., Wilde, F., Chapman, H. N. & Bajt, S. (2015). Rev. Sci. Instrum. 86, 125104. - PubMed
    1. Beyerlein, K. R., Dierksmeyer, D., Mariani, V., Kuhn, M., Sarrou, I., Ottaviano, A., Awel, S., Knoska, J., Fuglerud, S., Jönsson, O., Stern, S., Wiedorn, M. O., Yefanov, O., Adriano, L., Bean, R., Burkhardt, A., Fischer, P., Heymann, M., Horke, D. A., Jungnickel, K. E. J., Kovaleva, E., Lorbeer, O., Metz, M., Meyer, J., Morgan, A., Pande, K., Panneerselvam, S., Seuring, C., Tolstikova, A., Lieske, J., Aplin, S., Roessle, M., White, T. A., Chapman, H. N., Meents, A. & Oberthuer, D. (2017). IUCrJ, 4, 769–777. - PMC - PubMed