XRD enclosed chamber
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XRD Enclosed Chamber: This enclosed chamber enables real-time crystallization process investigations in reflection geometry within an X-ray diffractometer. Wide-angle diffraction measurements are taken over a 0° - 160° angular range, allowing for better and larger crystals to form inside the inner atmosphere of evaporation. The design is particularly suited for nanoparticles superlattices as well as proteins or other difficult-to-crystallize compounds. The chamber must be covered with a Kapton film that's transparent to X-rays. Its semicircular geometry ensures the X-ray beam always hits the Kapton perpendicularly, minimizing parasite scattering and absorption phenomena. Depending on the 3D printing material and Kapton used, the chamber will be compatible with various solvents. We tested PLA, which is compatible with water, alcohols, acetone, and tetrachloroethylene. However, it's not compatible with chloroform and dichloromethane. Our design has already been published in ACS Materials Letters, in a paper titled "Wide Angle X-Ray Diffraction Evidence of Structural Coherence in CsPbBr3 Nanocrystal Superlattices" by Toso et al. If you use this design for scientific purposes, please cite the publication: Toso, S., Baranov, D., Giannini, C., Marras, S., & Manna, L. Wide Angle X-Ray Diffraction Evidence of Structural Coherence in CsPbBr3 Nanocrystal Superlattices. ACS Mater. Lett. acsmaterialslett.9b00217 (2019). doi:10.1021/acsmaterialslett.9b00217 https://pubs.acs.org/doi/10.1021/acsmaterialslett.9b00217 Instructions: Print the chamber with 100% infill to prevent solvent loss or retention within porosities, using supports if needed. Once printed, insert a standard microscope glass slide on the bottom of the chamber as a cleanable and flat sample holder (cut it to approximately 15 x 49 x 1 mm). Then glue a Kapton film onto the top arched aperture, as shown in the illustration. Polyacrylate glue, such as Super-Attak, is suitable. Once the Kapton is glued in place, insert the spacer from below using the other aperture. It will fit without needing any glue and will push the chamber walls apart slightly. The chamber is now ready for use. Simply insert your sample inside and close the entrance aperture with another glass slide to provide non-sealed protection, allowing the solvent inside to slowly evaporate.
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